Day: November 24, 2020

188614-01-9. We know that the rate of many reactions can be accelerated by catalysts. A catalyst speeds up the rate of a reaction by lowering the activation energy; in addition, the catalyst is regenerated in the process. 188614-01-9, name is :Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate, below Introduce a new synthetic route.

188614-01-9, 3-Oxo-3, 4-dihydro-2H-benzo [1, 4] thiazine-6-carboxylic acid methyl ester (6.74 g) was suspended in tetrahydrofuran (100 ml) and 2M sodium hydroxide [(30] ml) was added followed by water (20 ml). The solution was stirred for 2.5 hours, evaporated to half volume and acidified with 2M hydrochloric acid. The product was collected, washed with water and dried in vacuo, to give a white solid (6.2 g). MS (-ve ion electrospray) [L} L/Z] 208 (M-H)-

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 188614-01-9, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; GLAXO GROUP LIMITED; WO2004/2992; (2004); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

The molecularity of an elementary reaction is the number of molecules that collide during that step in the mechanism., 154127-42-1, If there is only a single reactant molecule in an elementary reaction, that step is designated as unimolecular.154127-42-1, name is :(S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide. A new synthetic method of this compound is introduced below.

To a solution of IX (41 g, 0.12 moles) and triethylamine (33 ml. 0.24 moles) in anhydrous tetrahydrofuran (615 ml) cooled to 0 to 5 C. was added a solution of tosyl chloride (44 g, 0.24 moles) in tetrahydrofuran (205 ml). The mixture was allowed to warm to room temperature and stirred for 18 hours. The reaction mixture was cooled to 0 to 5 C. and ethylamine gas was purged from its 70% aqueous solution (365 ml) below 10 C. Reaction mixture was allowed to attain ambient temperature and stirred for 36 hours. The reaction mixture was concentrated and ethyl acetate (615 ml) was added to it. Further the organic layer was washed with water (410 ml). The concentrated ethyl acetate layer and MDC (615 ml) was added followed by cooling to temperature 0 to 5 C. and 6M hydrochloric acid (600 ml) was added. The reaction mixture was stirred for 1 h at 15 to 20 C. Aqueous layer was washed with MDC (205 ml). pH of the aqueous solution was adjusted to 8 using sodium bicarbonate solution causing white solid to precipitate which was extracted with ethyl acetate (2*410 ml). The ethyl acetate layer was evaporated to dryness to yield crude Brinzolamide (29 g, 66%). Material was recrystallized from ethanol. [Purity: greater than 99.5%, m.p. 125-127 C.], 154127-42-1

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,154127-42-1,(S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide,its application will become more common.

Reference£º
Patent; Sathe, Dhananjay Govind; Tarur, Radhakrishnan Venkatasubramanian; Bhise, Nandu Baban; Shinde, Ajit Bhaskar; Pardeshi, Santosh; US2010/9977; (2010); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A heterogeneous catalyst is a catalyst that is present in a different phase than the reactants. Such catalysts generally function by furnishing an active surface upon which a reaction can occur. 272437-84-0, name is :3-Oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylic acid, introduce a new downstream synthesis route as follows. 272437-84-0

3-Oxo-3,4-dihydro-2H-benzo[l,4]thiazine-6-carboxylic acid (31 mg, 0.14 mmol, 1.0 eq) is added at room temperature to a stirred solution of l-(6-methoxy-3,4-dihydro-2H-l-oxa-9-aza- phenanthrene-3-yl)-piperidin-4-ylamine (50 mg, 0.14 mmol, 1.0 eq) in N,N- dimethylformamide (3 mL), followed by 1-hydroxybenzotriazole (21 mg, 0.15 mmol, 1.1 eq), N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (31 mg, 0.16 mmol, 1.15 eq) and NN-diisopropylethylamine (53 mu, 0.31 mmol, 2.25 eq). After 15 hours stirring at room temperature, solvent is evaporated and the residue is extracted with dichloromethane (3 x 10 mL) and water (10 mL). The combined organic layers are dried over sodium sulfate, filtered and concentrated to give a crude product that is purified by preparative HPLC to afford 3-oxo-3,4- dihydro-2H-benzo[ 1 ,4]thiazine-6-carboxylic acid [ 1 -(6-methoxy-3 ,4-dihydro-2H- 1 -oxa-9- aza-phenanthrene-3-yl)-piperidin-4-yl] -amide as an off-white lyophilizated powder (24 mg, 33% yield). 1H-NMR (400 MHz, DMSO-dtf) delta ppm: 10.66 (br, 1H), 8.33 (s, 1H), 8.24 (d, J = 7.6 Hz, 1H), 7.81 (d, J = 9.0 Hz, 1H), 7.42 (m, 2H), 7.38 (m, 1H), 7.20 (m, 2H), 4.47 (d, J = 11.0 Hz, 1H), 4.02 (m, 1H), 3.93 (s, 3H), 3.78 (m, 1H), 3.50 (s, 2H), 3.20 (m, 1H), 3.08 (m, 2H), 3.00 (m, 2H), 2.42 (m, 2H), 1.81 (m, 2H), 1.58 (m, 2H).MS m/z (+ESI): 505.2 [M+H]+.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 272437-84-0.

Reference£º
Patent; BASILEA PHARMACEUTICA AG; GAUCHER, Berangere; DANEL, Franck, Hubert; TANG, XiaoHu; XIE, Tong; XU, Lin; WO2011/73378; (2011); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

188614-01-9. We know that the rate of many reactions can be accelerated by catalysts. A catalyst speeds up the rate of a reaction by lowering the activation energy; in addition, the catalyst is regenerated in the process. 188614-01-9, name is :Methyl 3-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylate, below Introduce a new synthetic route.

A. 3-Oxo-3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid. To a solution of 3-oxo-3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid methyl ester (1.5 g, 6,7 mmol) in a THF/H2O mixture (1:1, 63 mL) was added 4 N LiOH (8.0 mL, 32 mmol) and the resulting solution was stirred at RT for 24 h. The solution was partially concentrated and diluted with H2O (50 mL). The solution was acidified using concentrated HCl and a solid precipitated. The solid was collected via filtration, washed with H2O and dried in vacuo to provide 0.79 g (60%) of the title compound as a white solid. MS (ESI): exact mass calculated for C9H7NO3S, 209.01; m/z found, 210.2 [M+H]+. 1H NMR (500 MHz, CD3OD): 7.65-7.61 (m, 2H), 7.40 (d, J=8.1, 1H), 3.48 (s, 2H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 188614-01-9, and friends who are interested can also refer to it.

Reference£º
Patent; Allison, Brett D.; Gomez, Laurent; Grice, Cheryl A.; Hack, Michael D.; Morrow, Brian J.; Motley, S. Timothy; Santillan, Alejandro; Shaw, Karen J.; Schwarz, Kimberly L.; Tang, Liu Y.; Venkatesan, Hariharan; Wiener, John J. M.; US2006/223810; (2006); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.3080-99-7, name is :3,4-Dihydro-2H-benzo[b][1,4]thiazine. An updated downstream synthesis route of 3080-99-7 as follows.3080-99-7

(3d) Potassium carbonate (5.2 g, 37.7 mmol) and methyl 4-(bromomethyl)benzoate (2.8 g, 12.6 mmol) were added to a solution of (3c) (1.9 g, 12.6 mmol) in 20 mL of anhydrous DMF. The reaction mixture was heated to 80 C. overnight. After cooling to rt, the solid was filtered off and rinsed with DMF. The filtrate was concentrated in vacuo and the residue was purified on silica gel column to provide methyl 4-(2,3-dihydro-4H-1,4-benzothiazin-4-ylmethyl)benzoate (3.02 g, 80%).

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3080-99-7,3,4-Dihydro-2H-benzo[b][1,4]thiazine,its application will become more common.

Reference£º
Patent; Duan, Jingwu; Jiang, Bin; Chen, Lihua; Lu, Zhonghui; Barbosa, Joseph; Pitts, William J.; US2003/229084; (2003); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

154127-42-1. The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 154127-42-1, name is :(S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide

Prepare a 1L three-vial bottle equipped with a mechanical stirrer, a constant pressure low liquid funnel, and an ice water bath.Add compound of formula A (100 g, 0.28 mol) and acetonitrile (400 mL),Under N2 protection, stirring and cooling to 5 ~ 10 C,Then drop itTrimethyl orthoacetate(77.3g, 0.64mol),The rate of addition is such that the stability of the system does not exceed 15C.After the addition, remove the cooling and continue the reaction for 1 hour.TLC detected the disappearance of the starting material, creating a slightly more polar new point.Concentrate at normal pressure, recover the solvent and add the residue to DCM.Swirling to replace desolvation, and finally high vacuum drying for 1 hour,The residue is a compound of formula B-1Can be directly used in subsequent reactions without purificationThe reaction gave the crude product B-1 in equivalent yield.

The chemical industry reduces the impact on the environment during synthesis, 154127-42-1,(S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Shanghai Bo Shirui Life Technology Co., Ltd.; Wang Dong; Wang Fangdao; Wang Meng; Cai Maojun; (16 pag.)CN107722043; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

The molecularity of an elementary reaction is the number of molecules that collide during that step in the mechanism., 272437-84-0, If there is only a single reactant molecule in an elementary reaction, that step is designated as unimolecular.272437-84-0, name is :3-Oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylic acid. A new synthetic method of this compound is introduced below.

Preparation of (3-oxo-3,4-dihvdro-2H-benzori,41thiazine-6-carboxylic acid {trans-4-2-(6- methoxy-ri,51naphthyridin-3-yloxy)-ethyll-cvclohexyU)-amide: 3-Oxo-3,4-dihydro-2H-benzo[l,4]thiazine-6-carboxylic acid (59 mg, 0.25 mmol, 1.0 eq) is added at room temperature to a stirred solution of tralphar¡ã-4-[2-(6-methoxy- [l,5]naphthyridin-3-yloxy)-ethyl]-cyclohexylamine (80 mg, 0.25 mmol, 1.0 eq) inN,N- dimethylformamide (5 mL), followed by 1-hydroxybenzotriazole (37 mg, 0.28 mmol, 1.1 eq), N-(3-dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (56 mg, 0.29 mmol, 1.15 eq) and 7V,N-diisopropylethylamine (97 muL, 0.57 mmol, 2.25 eq). After 15 hours stirring at room temperature, solvent is evaporated and the residue is extracted with dichloromethane (3 x 10 mL) and water (10 mL). The combined organic layers are dried over sodium sulfate, filtered and concentrated to give a crude product that is purified by preparative EtaPLC to afford (3-oxo-3,4-dihydro-2H-benzo[l,4]thiazine-6-carboxylic acid {trans-4-[2-(6- methoxy-[l,5]naphthyridin-3-yloxy)-ethyl]-cyclohexyl})-amide as a white lyophilizated powder (36 mg, 27% yield). 1H-NMR (400 MHz, DMSO-t/6) delta ppm: 10.64 (s, IH), 8.53 (d, J = 2.8 Hz, IH), 8.19 (dd, J = 0.7, 9.0 Hz, 2H), 7.62 (dd, J = 0.5, 2.5 Hz, IH), 7.37-7.46 (m, 3H), 7.07 (d, J = 9.0 Hz, IH), 4.24 (t, J = 6.6 Hz, 2H), 4.00 (s, 3H), 3.70-3.80 (m, IH), 3.50 (s, 2H), 1.80-1.90 (m, 4H), 1.70-1.80 (m, 2H), 1.45-1.55 (m, IH), 1.30-1.40 (m, 2H), 1.05-1.18 (m, 2H). MS m/z (+ESI): 493.4 [M+H]+., 272437-84-0

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3-Oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylic acid,272437-84-0,its application will become more common.

Reference£º
Patent; BASILEA PHARMACEUTICA AG; GAUCHER, Berangere; DANEL, Franck Hubert; ROUSSEL, Patrick; WO2010/84152; (2010); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

154127-42-1. Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.154127-42-1, name is :(S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide, below Introduce a new synthetic route.

Compound B (50.0 g, 140.7 mmol) was added to 450 mL of acetonitrile, trimethyl orthoacetate (27.0 g, 225.1 mmol) and triethylamine (1.4 g, 14.0 mmol) were added with stirring, and the mixture was heated to 78C. , stirring for 5h,HPLC monitoring showed complete reaction and the HPLC monitoring results are shown in Table 1 (see FIG. 1).Cool to 40C, distill off under reduced pressure, and concentrate to a minimum volume.Compound C crude product was obtained.The crude compound C was dissolved in 180 mL of tetrahydrofuran, cooled to -10 DEG C, triethylamine (31.3 g, 309.5 mmol) was slowly added dropwise at a drip rate of 1 d/s, and the addition was completed at a drip rate of 3 d/s. 4- A solution of tosyl chloride (53.5 g, 280.6 mmol) in 70 mL of tetrahydrofuran. After the addition, the temperature was controlled at -4C, and the reaction was complete after about 3 hours.At a controlled temperature of 10 C. or less, a 70% aqueous solution of ethylamine (361.0 g, 5.6 M) was slowly added dropwise at a rate of 5 d/s. After the addition, the temperature was kept stirring at 12C and the reaction was complete after about 15 hours.The mixture was concentrated under reduced pressure to 70-80 mL, and the temperature was lowered to 0C. The temperature was controlled below 30C, and concentrated hydrochloric acid (12 mol/L) was added dropwise to adjust the pH to 1 to 2, and then about 14 mL of concentrated hydrochloric acid (12 mol/L) was added. The mixture was stirred at room temperature for 1 hour. The reaction was extracted twice with methyl tert-butyl ether (2*250 mL). The organic phases were combined and extracted once with dilute hydrochloric acid (1 mol/L, 100 mL). Combine the aqueous phases, slowly add sodium bicarbonate solids, adjust the pH to 5-6, add 150 mL of water, and adjust the pH to 7-8 with 7% sodium bicarbonate solution. After adjustment, stir at room temperature for 15 h and slowly crystallize. After filtration, the filter cake was rinsed with 30 mL of water and the cake was dried to obtain 35.4 g of product with a purity of 98.3%.Add 250 mL of dichloromethane, 25 mL of methanol to the filter mother liquor, stir, extract, separate, and concentrate the organic phase to dryness4.6 g of yellow viscous material was added and 10 mL of ethyl acetate was added. Heat to 70 ~ 75 C dissolved, slowly dropped to 0 ~ 10 C, stirring 1 ~ 2h, precipitation of a white solid, continue stirring 3 ~ 4h, filtration, with 3mL water filter cake, filter cake drying,Obtained product 2.4g, purity 97.3%.Combined, the purity was 98.1%, the total yield was 65.3%, the ignition residue was 0.08%, and the chiral purity was 99.7%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 154127-42-1, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; Shandong Weizhi Pharmaceutical Co., Ltd.; Shanghai Weizhi Pharmaceutical Technology Co., Ltd.; Wang Jianhua; He Yigang; Wei Yanjun; Xing Yanping; Zhao Tianchang; (27 pag.)CN107759618; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A heterogeneous catalyst is a catalyst that is present in a different phase than the reactants. Such catalysts generally function by furnishing an active surface upon which a reaction can occur. 37441-50-2, name is :1,2-Thiazinane 1,1-dioxide, introduce a new downstream synthesis route as follows. 37441-50-2

Part E 7-Bromo-2-ethoxymethyl-1-(3-isopropoxypropyl)-1FI imidazo[4,5-c]quinolin-4- amine (0.75 g), 1,4-butanesultam (0.29 g), copper (I) (68 mg), (No.)-trans-1,2- diaminocyclohexane (42 muL), potassium phosphate (0.79 g) and dioxane (4 mL) were added to a scintillation vial. The vial was flushed with nitrogen, sealed with a Teflon- lined cap, placed in an oil bath, and heated at 110 C for 30 hours. The reaction was cooled to ambient temperature, diluted with chloroform and filtered through a bed of CELITE filter agent. The solvent was evaporated and the residue was purified by column chromatography on a Biotage HorizonNo. High-Performance Flash Chromatography instrument using a silica gel cartridge. The polar component of the eluent was chloroform:methanol:ammonium hydroxide 80:18:2 (CMA). The purification was carried out eluting with chloroform: CMA in a gradient from 99: 1 to 90: 10. Additional purification by recrystallization from acetonitrile provided 0.47 g of 7-(1,1-dioxo- [1,2]thiazinan-2-yl)-2-ethoxymethyl-1-(3-isopropoxypropyl)-1H imidazo[4,5-c]quinolin- 4-amine as pale yellow crystals, mp 172-174 C., 37441-50-2

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 1,2-Thiazinane 1,1-dioxide.

Reference£º
Patent; 3M INNOVATIVE PROPERTIES COMPANY; WO2005/123080; (2005); A2;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

38642-74-9. We know that the rate of many reactions can be accelerated by catalysts. A catalyst speeds up the rate of a reaction by lowering the activation energy; in addition, the catalyst is regenerated in the process. 38642-74-9, name is :2-Cyano-phenothiazine, below Introduce a new synthetic route.

2-cyanophenothiazine (0.74 g, 3.30 mmol) was dissolved in 10 mL of anhydrous DMF. The mixture was cooled to 0 C and 60 % NaH (0.40 g, 9.90 mmol) was added. The dark mixture was stirred at 0 C for an additional 15 mm and Di-tert-butyl dicarbonate (0.90 g, 3.96 mmol) was added. The mixture was stirred at room temperature for 3 h and was diluted with 50 mL of brine. The aqueous layer was extracted with three 25 mL portions of ethyl acetate. The combined organic extract was dried over anhydrous MgSO4 and concentrated under diminished pressure. The crude was purified on a silica gel column (10 cm x 2 cm). Elution with ethyl acetate-hexane (1:9) gave 1 as a pale yellow solid: yield 1.07 g (100%); silica gel TLC R10.26 (ethyl acetate-hexane 1:9); ?HNIVIR (CDC13) 51.49 (s, 9H), 7.16-7.20 (m, 1H), 7.28-7.33 (m, 2H), 7.40 (s, 2H), 7.49 (d, 1H, J= 8.4 Hz) and 7.80 (s, 1H); ?3CI?IvIR 28.1, 83.1, 110.2, 118.2, 126.6, 127.2, 127.3, 127.5, 128.1,129.1, 130.3, 130.6, 137.7, 139.0, 139.1 and 151.8; mass spectrum (APCI), m/z 325.1017 (M+H) (C18H17N202S requires m/z 325.1011)., 38642-74-9

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 38642-74-9, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; ARIZONA BOARD OF REGENTS ON BEHALF OF ARIZONA STATE UNIVERSITY; HECHT, Sidney; KHDOUR, Omar; CHOWDHURY, Sandipan, Roy; BANDYOPADHAY, Indrajit; (85 pag.)WO2016/133995; (2016); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem