Day: October 28, 2020

92-39-7,Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2-Chloro-10H-phenothiazine,92-39-7, This compound has unique chemical properties. The synthetic route is as follows.

(1) Dehydration reaction: 2-chlorophenothiazine, cuprous cyanide, catalyst, quinoline, p-toluenesulfonyl chloride according to moleThe ratio is 1:1.25:0.15:5:0.1 is added to the reactor, and the temperature is raised to 120 C for dehydration reaction, the reaction is 1 hour, and the water is dehydrated to a moisture content of less than 0.1%;The catalyst is a mixture of sodium iodide and lithium iodide, and the molar ratio of sodium iodide to lithium iodide is 1:0.3;(2) Preparation of crude 2-cyanophenothiazine: the temperature of the reactor was raised to 230 C, and the reaction was carried out for 15 hours;(3) Separation of crude 2-cyanophenothiazine: the reactor temperature was lowered to 90 C, and 8 times was added to the reactor.The total amount of moles of the starting material is water, the solid is precipitated and filtered, and the product is extracted with ethyl acetate and concentrated to dryness to give a crude 2-cyanophenothiazine;(4) Purification of 2-cyanophenothiazine: a crude 2-cyanophenothiazine is placed in a mixed solvent of toluene and methanol,The volume ratio of toluene to methanol in the mixed solvent was 1:0.15, the temperature was raised to 120 C for 30 minutes, and the mixture was cooled to 20 C, and the precipitated solid was filtered to obtain 2-cyanophenothiazine.After testing, the yield of 2-cyanophenothiazine prepared in this example was 92.6%, and the purity of the product was 99.61%.The content of the amide was 0.03%.

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Reference£º
Patent; Ningbo Jinuo Chemicals Co., Ltd.; Peng Zhigang; Yue Mingxin; Qu Qiangzheng; (8 pag.)CN105175355; (2018); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.98827-44-2,A new synthetic method of this compound is introduced below.98827-44-2

260 kg of 4-hydroxy-2H-thieno [2,3-e] -1,2-thiazine-3-carboxylic acid methyl ester 1,1-dioxide were dissolved in500kgDMF, add potassium carbonate 150kg, warmed to 140 C, and dropping 120kg of dimethyl carbonate, 2h drop end, after the dropwise addition, the reaction was continued for 5h, then add 140kg of potassium carbonate, dropping 300 kg of 2 – aminopyridine in dimethylformamide (DMF) (120kg 2-aminopyridine dissolved in 180 kg DMF), 2h addition was complete, the reaction was continued for 5h. After the reaction, cooling and filtering to remove potassium carbonate, the filtrate was recovered under reduced pressure most of the DMF, the residue was added mass concentration of 3% sodium hydroxide alkaline water, activated carbon bleaching, filtration, the filtrate was purified hydrochloric acid to pH = 3 -4, precipitated yellowish solid, centrifuged, the material was washed until neutral, dried, to give a yellow solid 276kg, yield 83%, product purity 99.85%.

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Reference£º
Patent; Jiangsu Engineering Polytechnic College; Yan Bin; Feng Chengliang; Guo Liqiang; (5 pag.)CN106916169; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A common heterocyclic compound, 92-30-8,2-(Trifluoromethyl)-10H-phenothiazine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route. 92-30-8

To a solution of 2-(trifluoromethyl)-10H-phenothiazine (5.0g, 18.8mmol) and DMF (15mL) at RT was added finely powdered KOH (2.1g, 37.5mmol) and (¡À)-epibromohydrin (3.9mL, 48.9mmol). The reaction mixture was stirred at RT for 48h. Once no starting material was observed by analytical LCMS, EtOAC (250mL) and brine (250mL) were added. The organic layer was separated, and the aqueous layer was washed with EtOAC (3 chi lOOmL). The combined organic extracts were washed with brine (2 chi lOOmL), dried over MgSOzi, and concentrated to afford the title compound

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,92-30-8,2-(Trifluoromethyl)-10H-phenothiazine,its application will become more common.

Reference£º
Patent; INCEPTION 1, INC.; CHEN, Austin, Chih-Yu; SCOTT, Jill, Melissa; STEARNS, Brian, Andrew; STOCK, Nicholas, Simon; TRUONG, Yen, Pham; WO2013/43744; (2013); A2;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

A common heterocyclic compound, 3939-23-9,3-Bromo-10H-phenothiazine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route. 3939-23-9

Tri-tert-butylphosphine (4.4 mL of a 1.0 M solution in toluene, 1.48 g, 0.05 mmol), palladium acetate (0.4 g,1.83 mmol) and sodium tert-butoxide (52.7 g, 549 mmol) were added to 2-6-a (20.423 g, 73.42 mmol) and 2-6-c(11.53 g, 73.42 mmol) a solution in degassed toluene (500 mL), and the mixture was warmed under reflux for 2 hr.The reaction mixture was cooled to room temperature, diluted with toluene and filtered over EtOAc. Dilute the filtrate with water and use aThe benzene was extracted and the organic phases were combined and evaporated under vacuum. The residue was passed through silica gel (heptane / dichloromethane)Filtration was carried out and crystallized from isopropanol. Obtaining 2-6-b 19.51 g, yield 75%; the resulting bromide 2-6-b(7.89 g, 20 mmol), pinacol borate (6.22 g, 24 mmol), 1,1′-bis(diphenylphosphino)-ferrocene-palladium dichloride(II) dichloromethane complex (0.49 g, 0.6 mmol), potassium acetate (5.90 g, 60 mmol) and 79 ml of toluene were reacted under refluxAfter 16 hours, cool, add 26 ml of water and stir for 30 minutes.The organic phase is separated and filtered through a short bed of diatomaceous earth, followed by organicThe solvent was distilled off and the crude product was recrystallized from heptane / toluene.The compound 2-6 was obtained in an amount of 6.58 g, yield 82%.

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,3939-23-9,3-Bromo-10H-phenothiazine,its application will become more common.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Zhang Hong; Cai Hui; (36 pag.)CN108530418; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Adding a certain compound to certain chemical reactions, such as: 272437-84-0,3-Oxo-3,4-dihydro-2H-1,4-benzothiazine-6-carboxylic acid, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 272437-84-0,272437-84-0

B. 6-Hydroxymethyl-4H-benzo[1,4]thiazin-3-one. To a 0 C. suspension of 3-oxo-3,4-dihydro-2H-benzo[1,4]thiazine-6-carboxylic acid (400 mg, 2 mmol) in THF (19 mL) was added Et3N (0.32 mL, 2 mmol) and the resulting solution was treated with iso-butylchloroformate (0.3 mL, 2 mmol). The resulting suspension was stirred at 0 C. for 2 h, filtered and the solid was washed with THF. The filtrate was cooled to 0 C., treated with NaBH4 (150 mg, 4.3 mmol) and slowly treated with H2O (10 mL). The resulting suspension was, warmed to RT and stirred for 18 h. The suspension was neutralized using 1 N HCl and diluted with H2O (100 mL). The organic layer was extracted with EtOAc (3*200 mL). The combined organic layers were dried (MgSO4), filtered and concentrated. The resulting residue was purified on SiO2 (0-10% CH3OH/CH2Cl2) to provide 330 mg (89%) of the title compound as a white solid. MS (ESI): exact mass calculated for C9H9NO2S, 195.04; m/z found, 196.1 [M+H]+. 1H NMR (500 MHz, CD3OD): 7.26 (d, J=7.9, 1H), 7.01-6.98 (m, 2H), 4.55 (s, 2H), 3.40 (s, 2H).

According to the analysis of related databases, 272437-84-0, the application of this compound in the production field has become more and more popular.

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

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 1,2-Thiazinane 1,1-dioxide,37441-50-2, This compound has unique chemical properties. The synthetic route is as follows.,37441-50-2

8-HYDROXY- [1, 6] naphthyridine-7-carboxylic acid methyl ester 1A. 4 (WO 0230930 A2, p. 171) is reacted with one molar equivalent of N-bromosuccinimide in dichloromethane, to yield 5-BROMO-8-HYDROXY- [1, 6] NAPHTLIYRIDINE-7-CARBOXYLIC acid methyl ester, 1A. 5. The phenol is then reacted with p-toluenesulfonyl chloride and triethylamine in CHLOROFONN, FOR example as described in WO 02 30931 A2 p. 72, to give 5-bromo-8- (toluene-4-sulfonyloxy)- [1, 6] naphthyridine-7-carboxylic acid methyl ester 1A. 6. The product is then reacted with [1, 2] thiazinane 1, 1-dioxide 1A. 7 and cuprous oxide in pyridine at reflux, for example as described in WO 0230931 A2, p. 73, to produce 5- (1, 1-DIOXO- 1,2] thiazinan-2-yl)-8- (toluene-4-sulfonyloxy)- [1, 6] naphthyridine-7-carboxylic acid methyl ester 1A. 8. Deprotection, for example by reaction with methanol sodium methoxide in DIMETHYLFORMAMIDE, as described in WO 0230931 A2 p. 74, then affords the phenol 1A. 9.

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 37441-50-2.

Reference£º
Patent; GILEAD SCIENCES, INC.; WO2005/28478; (2005); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3939-23-9,3-Bromo-10H-phenothiazine, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.3939-23-9

2, under nitrogen protection will be prepared in step 1 p-phenylenediamine and phenothiazine derivatives according to 1:1 molar ratio was added to toluene, while adding potassium tert-butyl alcohol and palladium acetate as a catalyst,The reaction was heated to 80 C for 3 hours and then cooled to room temperature. The reaction was filtered,The filtrate was washed with dichloromethane and then the solvent was evaporated to dryness. The crude product was repeatedly washed with methanol and acetone,The product is obtained after purification by column chromatography., 3939-23-9

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 3-Bromo-10H-phenothiazine.

Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Guo Jianhua; (12 pag.)CN106831645; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. (S)-4-Hydroxy-2-(3-methoxypropyl)-3,4-dihydro-2H-thieno[3,2-e][1,2]thiazine-6-sulfonamide 1,1-dioxide,154127-42-1, This compound has unique chemical properties. The synthetic route is as follows.,154127-42-1

Step J: (+)-4-Ethylamino-3,4-dihydro-2-(3-methoxy)propyl-2H-thieno[3,2-e]-1,2-thiazine-6-sulfonamide-1,1-dioxide hydrochloride To a solution of the product from Step I (2.4 g, 6.74 mmol) and triethylamine (3.8 mL, 27 mmol) in anhydrous tetrahydrofuran (20 mL) cooled to -20 C. was added tosyl chloride (2.6 g, 13.5 mmol); this mixture was allowed to warm to room temperature and stirred for 18 hr. The reaction mixture was cooled to -60 C. and ethylamine (10 mL) was added and the mixture was again allowed to warm to room temperature. After 18 hr the reaction mixture was diluted with ethyl acetate (200 mL), washed with a saturated aqueous solution of sodium bicarbonate (3*50 mL), dried (MgSO4), and evaporated to give the crude product which was purified by column chromatography [silica; CH3 OH/CH2 Cl2 (20:1)] to give 1.3 g (52%) of the desired amine. The free base was dissolved in ethanol (5 mL) and treated with a 2M solution of hydrochloric acid in ethanol (4 mL) at room temperature. Evaporation of the solvent provided a solid which was recrystallized from methanol: methylene chloride to give 950 mg (34%) of the desired product; mp 175-177 C.; [~]D +10.35 (C=1.00, H2 O). Analysis. Calculated for C12 H22 ClN3 O5 S3: C, 34.32; H, 5.28; N, 10.00 Found: C, 34.26; H, 5.23; N, 9.92., 154127-42-1

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 154127-42-1.

Reference£º
Patent; Alcon Laboratories, Inc.; US5378703; (1995); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

37441-50-2,A common heterocyclic compound, 37441-50-2,1,2-Thiazinane 1,1-dioxide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

Intermediate 524-Fluoro- 2-(l,l-dioxo-llambda6-[l,2]thiazinan-2-yl)benzonitrile: To a solution of l,l-dioxo[l,2]thiazinane (8.84 g, 65.4 mmol) in DMF (20 mL) and THF (10 mL) was added portion-wise sodium hydride (1.65 g, 65.5 mmol, 95%). After stirring for 30 min, 2,4-difluorobenzonitrile (10.0 g, 72 mmol) was added and the mixture was stirred at 90 C for 2.5 h. The mixture was cooled and concentrated and the residue was purified by flash chromatography eluting with 0%-l 0% EtOAc/hexane to give the title compound as white needles (1.37 g, 8% yield). 1H-NMR (500 MHz, CDCl3) delta: 7.70 (IH, dd, J= 8.8, 5.8 Hz), 7.30 (IH, dd, J= 8.8, 2.4 Hz), 7.15-7.12 (IH, m), 3.72 (2H, t, J= 5.3 Hz), 3.33 (2H, t, J= 6.1 Hz), 2.40-2.35 (2H, m), 2.05-2.01 (2H, m). LCMS [M+H]+ calcd for C11H12N2FO2S: 255.06; found: 255.19.

The chemical industry reduces the impact on the environment during synthesis, 37441-50-2,1,2-Thiazinane 1,1-dioxide,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2007/58646; (2007); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.3080-99-7,A new synthetic method of this compound is introduced below.3080-99-7

To a round bottom flask charged with compound 16-1 (151 mg, 1.0 mmol) and methyl 4-(bromomethyl)benzoate (228 mg, 1.0 mmol) in DMF (5 mL) was added K2CO3 (276 mg, 2.0 mmol). The resulting mixture was allowed to stir for 2 h at 80 C. The mixture was cooled to room temperature and after addition of water (15 mL) extracted with EtOAc (3 x 15 mL). The combined organic extracts were washed with brine (20 mL), dried over sodium sulfate, and concentrated under vacuum. The crude product was purified by flash chromatography (0 – 50% EtOAc/hexanes) to afford as colorless oil (110 mg, 37%).1H NMR (CDCI3) delta 8.00, 7.33 (AlphaAlpha’ChiChi’ multiplet, AX + J AX = 8.4 Hz, 4H), 7.08 (dd, / = 7.7 Hz, 1.5 Hz, 1H), 6.90 (incompletely resolved ddd approaching dt, average of two larger / = 7.8 Hz, additional / = 1.1 Hz, 1H), 6.63 (incompletely resolved ddd approaching dt, average of two larger / = 7.5 Hz, additional / = 0.8 Hz, 1H), 6.54 (dd, 7 = 8.3 Hz, 0.7 Hz, 1H), 4.57 (s, 2H), 3.90 (s, 3H), 3.69, 3.08 (AlphaAlpha’ChiChi’ multiplet, AX + J AX = 10.4 Hz, 4H). 13C NMR (CDCI3) delta 166.9, 143.8, 143.4, 130.1 (2C), 129.1, 128.0, 126.6 (2C), 126.1, 118.0, 117.8, 113.2, 56.3, 52.1, 50.6, 25.9. ESI LRMS: [M+H]+, mlz 300.2., 3080-99-7

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Reference£º
Patent; THE BOARD OF TRUSTEES OF THE UNIVERSITY OF ILLINOIS; KOZIKOWSKI, Alan; SHEN, Sida; BERGMAN, Joel; (100 pag.)WO2017/142883; (2017); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem