Derivation of elementary reaction about 92-30-8

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Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.92-30-8, name is :2-(Trifluoromethyl)-10H-phenothiazine, below Introduce a new synthetic route.. 92-30-8

II-4 (20g, 75mmol) a 100mL reaction flask was added DMF (60mL) was stirred and dissolved, was added potassium carbonate (15.5g, 113mmol), stirred at 60¡ãC , portionwise Intermediate III-5 (17.5g , 79mmol), the reaction after 1h, TLC analysis showed completion of the reaction (developing solvent, ethyl acetate: petroleum ether = 1: 3). The reaction solution was poured into 200ml cold water, with stirring, solid precipitated out.Filter cake was washed with water, and dried to give brown crude solid.The crude product was recrystallized from ethanol to give slightly yellow solid 30.0g. Purity 98.8percent (HPLC normalization method), a yield of 88.3percent.ESI-MS ([M + H] +): 453.0.

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Reference£º
Patent; Tianjin Pharmaceutical Institute Co., Ltd.; Liu Ying; Liu Dengke; Mu Shuai; Yue Nan; Gong Min; Zhi Shuang; Liu Changxiao; (25 pag.)CN104230848; (2017); B;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Discovery of Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, and friends who are interested can also refer to it.

98827-44-2. 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. 98827-44-2, name is :Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, introduce a new downstream synthesis route as follows.

5.3 g of TNXK-3 and 20 ml of methanol were added to a reaction flask. Stir at room temperature. Separately add dimethyl sulfate 3.7 g methanol (5 ml) solution and 50% sodium hydroxide solution (5 ml). After the completion of the dropping, room temperature reaction 3 hours, cooling to 10 degrees, the water 50 ml dilution, use 10% hydrochloric acid to the PH is 3. Filtering, the filter cake after the water washing, drying, recrystallization with methanol, 60 degrees decompression drying, getting white solid 4.8 g, yield 86%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide, and friends who are interested can also refer to it.

Reference£º
Patent; Jiangxi Yong Tong Technology Co., Ltd.; Liu Zhongchun; (13 pag.)CN107141308; (2017); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Extended knowledge of Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide

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. 98827-44-2, other downstream synthetic routes, hurry up and to see.

98827-44-2, The molecularity of an elementary reaction is the number of molecules that collide during that step in the mechanism. If there is only a single reactant molecule in an elementary reaction, that step is designated as unimolecular.98827-44-2, name is :Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide. 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%.

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. 98827-44-2, other downstream synthetic routes, hurry up and to see.

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

 

Little discovery in the laboratory: a new route for 1,2-Thiazinane 1,1-dioxide

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37441-50-2. An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.¡¾CAS/Name¡¿.Here is a downstream synthesis route of the compound 37441-50-2, name is :1,2-Thiazinane 1,1-dioxide

A stirred mixture of methyl 6-BROMO-3-HYDROXYPYRIDINE-2-CARBOXYLATE (6.15 g, 26.5 mmol), 8-sultam (described in WO 02/30931-A2, Merck & Co. , Inc. , 2002) (3. 98 g, 29.4 mmol) and copper (I) oxide (5.75 g, 40.2 mmol) in anhydrous pyridine (100 mL) was heated at 130 C, under argon, for 6 h. The mixture was cooled, and the pyridine removed under reduced pressure. The residue was treated with CH2C12 (400 mL) and EDTA (0.35 M in H20, 300 ML, 105 mmol) and air was bubbled into the mixture for 18 h. The mixture was filtered through a pad of celite and the aqueous layer was saturated with solid NACI and extracted with CH2CLZ (4 x 250 mL). The combined organic extracts were dried (NA2S04), filtered, and concentrated in vacuo to afford a crude oil. The oil was dissolved in MEOH (400 mL) and conc. H2S04 (2 ML) and heated to reflux for 18 h, then allowed to cool to ambient temperature. Most of the solvent was removed in vacuo and the residual mixture was partitioned between CHZCLX (400 mL) and saturated NAHCO3 (400 mL). The aqueous layer was extracted further with CH2Cl2 (2 x 250 mL) and the combined organic extracts were dried (NA2S04), filtered, and concentrated in vacuo to afford a crude sample of the product. This crude product was partially purified by silica gel chromatography, eluting with a gradient of CH2C12 : MEOH-100 : 0 to 95: 5 to give a yellow solid that was crystallized from MEOH to afford the title compound as a pale yellow solid of sufficient purity for use in the next step. MS: FALZ = 287 (M + 1).

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Reference£º
Patent; MERCK & CO., INC.; WO2005/9962; (2005); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Sources of common compounds: 2-(Trifluoromethyl)-10H-phenothiazine

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The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, 92-30-8, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 92-30-8, name is :2-(Trifluoromethyl)-10H-phenothiazine

General procedure: To a mixture of sodium hydride suspension (60percent, 0.26 g, 6.67 mmol) and phenothiazine derivative in abs. THF (50 cm3) was added the appropriate 3-aryltetrazolo[1,5-a]pyridin-4-ium tetrafluoroborate (1) in portions over 20 min, and the mixture was stirred at room temperature for 2 days. After evaporation of the reaction mixture, the residue was dissolved in a 1:1 mixture of EtOAc:water (50 cm3) and the solid product was filtered off. The aqueous mother liquor was extracted with EtOAc (thrice) and the organic phase was dried over anhydrous Na2SO4, filtered and evaporated. The combined organic solvent was evaporated, the residue was washed with diethyl ether then it was recrystallized from ethyl acetate – unless otherwise stated – to give the product.

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Reference£º
Article; Taka?cs, Daniella; Nagy, Ildiko?; Bombicz, Petra; Egyed, Orsolya; Jemnitz, Katalin; Riedl, Zsuzsanna; Molna?r, Jo?zsef; Amaral, Leonard; Hajo?s, Gyo?rgy; Bioorganic and Medicinal Chemistry; vol. 20; 14; (2012); p. 4258 – 4270;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Little discovery in the laboratory: a new route for 1,2-Thiazinane 1,1-dioxide

According to the analysis of related databases, 1,2-Thiazinane 1,1-dioxide, the application of this compound in the production field has become more and more popular.

37441-50-2. An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.¡¾CAS/Name¡¿.Here is a downstream synthesis route of the compound 37441-50-2, name is :1,2-Thiazinane 1,1-dioxide

To a mixture of 2,4-difluorobenzonitrile (10.0 g, 72 mmol) and 1,1-dioxo-1?6-[1,2]thiazin-2-ane (8.84 g, 65.4 mmol) in 1:1 tetrahydrofuran/dimethylformamide (40 mL) was added potassium carbonate (9.0 g, 65.4 mmol). The mixture was stirred at 90 C. for 18 h then filtered and concentrated. The residue was purified by flash chromatography (SiO2) eluting with 10%-50% ethyl acetate/hexanes followed by recrystallization from hot ethyl acetate/hexane to give the title compound as white needles (0.537 g, 3% yield). 1H NMR (500 MHz, CD3OD) ? ppm: 7.70 (1H, dd, J=8.8, 5.8 Hz), 7.30 (1H, dd, J=8.8, 2.4 Hz), 7.15-7.12 (1H, m), 3.27 (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 C11H16N2OF: 255.06; found: 255.19.

According to the analysis of related databases, 1,2-Thiazinane 1,1-dioxide, the application of this compound in the production field has become more and more popular.

Reference£º
Patent; Naidu, B. Narasimhulu; Banville, Jacques; Beaulieu, Francis; Connolly, Timothy P.; Krystal, Mark R.; Matiskella, John D.; Ouellet, Carl; Plamondon, Serge; Remillard, Roger; Sorenson, Margaret E.; Ueda, Yasutsugu; Walker, Michael A.; US2005/267105; (2005); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Flexible application of 1,2-Thiazinane 1,1-dioxide in synthetic route

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.

An elementary termolecular reaction involves the simultaneous collision of three atoms, 37441-50-2, molecules, or ions. Here is a downstream synthesis route of the compound 37441-50-2, name is :1,2-Thiazinane 1,1-dioxide

To a mixture of 2,4-difluorobenzonitrile (10.0 g, 72 mmol) and 1,1-dioxo-1lambda6-[1,2]thiazin-2-ane (8.84 g, 65.4 mmol) in 1:1 tetrahydrofuran/dimethylformamide (40 mL) was added potassium carbonate (9.0 g, 65.4 mmol). The mixture was stirred at 90 C. for 18 h then filtered and concentrated. The residue was purified by flash chromatography (SiO2) eluting with 10%-50% ethyl acetate/hexanes followed by recrystallization from hot ethyl acetate/hexane to give the title compound as white needles (0.537 g, 3% yield). 1H NMR (500 MHz, CD3OD) delta ppm: 7.70 (1H, dd, J=8.8, 5.8 Hz), 7.30 (1H, dd, J=8.8, 2.4 Hz), 7.15-7.12 (1H, m), 3.27 (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 C11H16N2OF: 255.06; found: 255.19., 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 37441-50-2.

Reference£º
Patent; Bristol-Myers Squibb Company; US2007/111984; (2007); A1;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Little discovery in the laboratory: a new route for 2-Methoxyphenothiazine

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 1771-18-2.

An elementary termolecular reaction involves the simultaneous collision of three atoms, 1771-18-2, molecules, or ions. Here is a downstream synthesis route of the compound 1771-18-2, name is :2-Methoxyphenothiazine

Step a 4-(3′-indolyl)-1-[1″-(2′”-methoxy-10′”-phenothiazinyl) -2″-methyl-3″-propionyl]-piperidine hydrochloride A mixture of 23 g of 2methoxy-phenothiazine, 21 g of methacryloyl chloride and 120 ml of toluene was refluxed for 3 hours and was then cooled and washed with 250 ml of N sodium hydroxide. The organic phase was decanted and the aqueous phase was washed twice with 50 ml of toluene. The combined organic phases were washed with water, dried over magnesium sulfate, treated with carbon black and evaporated to dryness to obtain 29.6 g of 2-methoxy-10-(alpha-methyl acryloyl)-phenothiazine melting at 91-92 C., 1771-18-2

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 1771-18-2.

Reference£º
Patent; Roussel-UCLAF; US3988453; (1976); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

The effect of 1,2-Thiazinane 1,1-dioxide reaction temperature change on equilibrium

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.

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

solution of 2-(3-chloro-4-fluorobenzyl)-8-ethyl-4-fluoro-10-methoxy-6-methyl-7,8- dihydropyrazino[l’,2′: 1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (0.10 g, 0.23 mmol; Example 139), 1,2-thiazinane 1,1-dioxide (45 mg, 0.33 mmol), and cesium carbonate (0.15 g, 0.46 mmol) in anhydrous DMSO (9.5 mL) was heated in an oil bath at 50 C for 5 hours. The product mixture was filtered through a pad of Celite and the filtrate was subjected to purification on reverse phase preparative HPLC purification. Collection and lyophilization of appropriate fractions afforded the title material. Analytical HPLC indicated that the product is a 1:1 mixture of two isomers that arose from the relative stereochemistry of the 6-methyl group and restricted rotation between the sultam ring and the tricyclic core. ?H NMR (400 MHz, CDCI3) No. 7.48 (m 1H), 7.28 (m, 1H), 7.11 (t, J = 8.5 Hz, 1H), 5.17 (d, J = 14.2 Hz, ?H), 5.34 (in, 1/2 H), 5.29 (d, J = 14.2 Hz, (at)H), 5.23 (d, J = 14.2 Hz, ?H), 5.09 (d, J = 14.2 Hz, ?H), 5.07 (m, ?H), 4.18 (s, 1.5H), 4.16 (s, 1.5H), 4.12-3.17 (m), 2.58-2.00 (m), 1.57 (d, J = 6.6 Hz, 1.5H), 1.42 (d, J = 6.8 Hz, 1.5H), 1.23 (t, J = 6.8 Hz, 1.5H), 1.22 (t, J = 7.1 Hz, 1.5H). ES MS M+1 = 552, 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 37441-50-2.

Reference£º
Patent; MERCK & CO., INC.; WO2005/110414; (2005); A2;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem

 

Research on new synthetic routes about Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide

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98827-44-2, 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.98827-44-2, name is :Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide. An updated downstream synthesis route of 98827-44-2 as follows.

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%.

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, Methyl 4-hydroxy-2H-thieno[2,3-e][1,2]thiazine-3-carboxylate 1,1-dioxide.

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