Day: August 26, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.111248-89-6,1,3-Dihydrobenzo[c]isothiazole 2,2-dioxide,as a common compound, the synthetic route is as follows.

To a suspension of 1 ,3-dihydrobenzo[c]isothiazole-2,2-dioxide (280 mg, 1.655 mmol) and potassium carbonate (229 mg, 1.66 mmol) in DMF (5 mL) was added iodomethane (414 pL, 6.62 mmol). The reaction was stirred for 6 h at RT and was then quenched with a saturated solution of ammonium chloride. The reaction mixture was concentrated and purified by column chromatography (cyclohexane/acetone) to afford the title compound as a white solid (270 mg, 89%). 1H NMR (500 MHz, CDCl3) ppm = 7.37 – 7.32 (m, 1 H), 7.27 – 7.24 (m, 1 H), 7.02 (td, J=7.6, 1.0, 1 H), 6.73 (d, J=8.0, 1 H), 4.34 (s, 2H), 3.14 (s, 3H). Rt = 2.07 min (HPLC method C).

As the paragraph descriping shows that 111248-89-6 is playing an increasingly important role.

Reference£º
Patent; MERCK PATENT GMBH; CANCER RESEARCH TECHNOLOGY LIMITED; SCHIEMANN, kai; STIEBER, Frank; BLAGG, Julian; MALLINGER, Aurelie; WAALBOER, Dennis; RINK, Christian; CRUMPLER, Simon Ross; WO2014/63778; (2014); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

288-16-4, Isothiazole is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Compound 1 (20 g, 0.235 mol) was added under stirring with nitrogen to dry 100 ml of ether and stirred and dissolvedThe temperature is 0 C or lower, n-butyllithium (0.24 mol) is added dropwise thereto, and the mixture is kept at 0 C or lower during the dropwise addition.Temperature reaction until no compound 1.To the reaction solution was added dropwise bromine (0.5 mol), and the mixture was kept below 0 C during the dropwise addition, and the mixture was gradually raised toAfter stirring for half an hour, the reaction was quenched by adding hydrochloric acid solution (2N, 500 ml) thereto.And the aqueous phase was extracted with ether (200 ml * 3) and discarded. The organic phase was combined and washed with sodium dithionite solution(100 ml * 2), dried over anhydrous sodium sulfate, filtered and concentrated to dryness to give compound 2 as a yellow oil.

288-16-4 Isothiazole 67515, aisothiazole compound, is more and more widely used in various.

Reference£º
Patent; Tianjin Jinyao Group Co., Ltd.; Li Jing; He Guangjie; Yang Xinyi; Wang Shuli; Chen Liying; Hu Xiaoyun; Sun Liang; (38 pag.)CN106890180; (2017); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

4576-90-3, Isothiazole-3-carboxylic acid is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a stirred solution compound 40 (3 g, 23.25 mmol) in CH2Cl2 (60 mL) under inert atmosphere were added EDCI.HCl (4.9 g, 25.58 mmol), DMAP (2.8 g, 23.25 mmol), N- methylmorpholine (7.65 mL, 69.76 mmol) and N, O-dimethylhydroxylamine hydrochloride (2.72 g, 27.90 mmol) at 0 oC, followed by warming to room temperature and stirring for 16 h. The reaction was monitored by TLC. After completion of the reaction, the reaction mixture was diluted with ice-cold water and extracted with CH2Cl2. The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to obtain the crude. The crude was purified through silica gel flash column chromatography using 40-45% EtOAc/ hexanes to afford compound 41 (2.5 g, 63%) as brown syrup. TLC: 40% EtOAc/ hexanes (Rf: 0.5); 1H NMR (400 MHz, DMSO-d6): delta 9.15 (d, J = 4.8 Hz, 1H), 7.63 (d, J = 4.4 Hz, 1H), 3.69 (s, 3H), 3.33 (s, 3H); LCMS Calculated for C6H7NOS: 141.02; Observed: 142.0 (M+1)+.LC-MS: 98.67%; 172.9 (M+1)+.

The synthetic route of 4576-90-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; ASSEMBLY BIOSCIENCES, INC.; TURNER, William, W., Jr.; LI, Leping; HAYDAR, Simon, Nicolas; BURES, Mark, G.; RAI, Roopa; FRANCIS, Samson; ARNOLD, Lee, Daniel; (0 pag.)WO2018/160878; (2018); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

87691-88-1, 3-Piperazinobenzisothiazole hydrochloride is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5. Preparation of ZPR in the melt of Na C03 decahydrate. To the melt of Na2C03 decahydrate (40g) was added BITP HCl (lOg) and CEI (10.35g) and the mixture was heated at 95 C for 10 hours. After 10 h the conversion to ZRP was 88. 2% (% area by HPLC). To the reaction mixture water was added and the solid was filtrated and washed with water. After drying the solid weighs 17.14g (purity by HPLC 88%).; 7. Preparation of ZPR in the presence of NaCl. In a three necked flask was charged 40 ml brine, BITP HC1 (14. 1g), CEI (10.35g) and Na2C03 (14. 1g) ; the mixture was than heated at 90C for 16hours. After this the mixture was cooled, water was added and the solid was filtrated, washed with water and dried. The product weights after drying 16.9g (purity by HPLC 87.5%).

As the paragraph descriping shows that 87691-88-1 is playing an increasingly important role.

Reference£º
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2005/40160; (2005); A2;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

288-16-4, Isothiazole is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 1 alpha,alpha-Bis(4-chlorophenyl)-5-isothiazolemethanol To a solution of 1.0 g of isothiazole in 20 ml of tetrahydrofuran were added 8.1 ml of a 1.52M solution of n-butyllithium in hexane at -78 C. The mixture was allowed to stir for 15 minutes at which time 3.2 g of 4,4′-dichlorobenzophenone were added as a solution in 25 ml of tetrahydrofuran. The reaction was allowed to warm to room temperature and was stirred for 2 hours. Twenty-five milliliters of a saturated ammonium chloride solution were added and the tetrahydrofuran was removed by evaporation. The resulting mixture was extracted three times with ethyl acetate. The combined organic extracts were washed with a saturated ammonium chloride solution, water, and a saturated sodium chloride solution, dried over magnesium sulfate and evaporated. The resulting oil was chromatographed over silica gel. The appropriate fractions were combined and evaporated resulting in an oil. Cyclohexane was added and 1.21 g of the desired title product were recovered by filtration as white crystals, m.p. 118-119.5 C. Analysis for C16 H11 Cl2 NOS: Calc.: C, 57.15; H, 3.30; N, 4.17; Found: C, 57.17; H, 3.07; N, 4.17.

The synthetic route of 288-16-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; Eli Lilly and Company; US4560695; (1985); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.24340-77-0,4-Bromoisothiazole,as a common compound, the synthetic route is as follows.

10456] 0.150 g (0.67 mmol) of 2-[6-(1H-pyrazol-4-yl)py- ridin-2-yl]pyrimidine (cf. Step 3) were initially charged, and 0.350 g (1.07 mmol) of caesium carbonate, 4.81 mg (0.03 mmol) of copper(I) oxide, 18.4mg (0.13 mmol) of salicylaldoxime, 0.165 g (1.0 mmol) of 4-bromoisothiazole and 1 ml of N,N-dimethylformamide were added successively under argon. The reaction mixture was heated at 110 C. for 24 hours. After cooling, the solvent was removed on a rotary evaporator under reduced pressure and the residue was purified by medium pressure column chromatography (MPLC) with cyclohexane/acetone (100:0 to 0:100). This gave 4.7mg (2% of theory) of2-{6-[1 -(isothiazol-4-yl)-1 H-pyrazol-4-yl] pyridin-2-yl}pyrimidine.10457] HPLC-MS: log P (HCOOH)=1.65, log P (neutral)=1.64.

As the paragraph descriping shows that 24340-77-0 is playing an increasingly important role.

Reference£º
Patent; BAYER CROPSCIENCE AG; Koehler, Adeline; Bretschneider, Thomas; Muehlthau, Friedrich August; Fuesslein, Martin; Jeschke, Peter; Fischer, Reiner; Voerste, Arnd; Malsam, Olga; Ilg, Kerstin; US2015/284380; (2015); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

4576-90-3, Isothiazole-3-carboxylic acid is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a stirred suspension of isothiazole-3-carboxylic acid (10.02 g, 77.6 mmol) in anhydrous te/f-butanol (80 ml_) and anhydrous toluene (120 ml_) was slowly added triethylamine (13.0 ml_, 93.12 mmol). The mixture was stirred at ambient temperature for 5 minutes and then diphenyl phosphoryl azide (18.42 ml_, 85.36 mmol) was added dropwise to it. The reaction mixture was stirred at ambient temperature for 1 h, gradually warmed to 85 C over 1 h, and then heated at 85 C with stirring for 7 h. After cooling to ambient temperature, the reaction mixture was diluted with ethyl acetate (150 ml_) and saturated aqueous sodium bicarbonate (150 ml_). The layers were separated and the aqueous layer was extracted with ethyl acetate (2 c 100 ml_). The combined organic layers were washed with water (150 ml_), brine (150 ml_), dried over magnesium sulfate, and filtered. Concentration of the filtrate in vacuo provided a residue, which was purified by column chromatography, eluting with a gradient of 0 to 10% of ethyl acetate in heptane. Further purification by column chromatography, eluting with a gradient of 0 to 10% of ethyl acetate in dichloromethane, afforded the title compound as a colorless solid (10.33 g, 66% yield): 1H NMR (400 MHz, CDCI3) d 8.56 (dd, J = 4.9, 0.6 Hz, 1 H), 8.11 (s, 1 H), 7.66 (d, J = 4.9 Hz, 1 H), 1.53 (s, 9H); MS (ES+) m/z 201.1 (M + 1).

The synthetic route of 4576-90-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; XENON PHARMACEUTICALS INC.; FOCKEN, Thilo; BURFORD, Kristen Nicole; LOFSTRAND, Verner Alexander; WILSON, Michael Scott; ZENOVA, Alla Yurevna; (121 pag.)WO2019/241533; (2019); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

24340-77-0, 4-Bromoisothiazole is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

a) 6- (Isothiazol-4-yl)-8- ((2- (trimethylsilyl)ethoxy)methoxy)-3- ((2- (trimethylsilyl)ethoxy)methyl)guinazolin-4(3H)-oneA suspension of 4-bromo-isothiazole (0.02 g, 0.1 mmol), (6- (4,4,5 ,5-tetramethyl- 1,3,2- dioxaborolan-2-yl)-8- ((2- (trimethylsilyl)ethoxy)methoxy)-3-((2-(trimethylsilyl)ethoxy)methyl)quinazolin-4(3H)-one (0.05 g, 0.08 mmol, example 28), bis (diphenylphosphino)feffocene-palladium(II)dichloride (0.01 g, 0.01 mmol), potassium carbonate (0.03 g, 0.25 mmol) and water (0.2 ml) in dimethylformamide (1 ml) was stirred in a sealed tube at 100 C for 2 hours and then at 80 C overnight. Filtration and chromatography (C18 reverse phase HPLC, methanol / water (0.1% formic acid) = 40:60 to 100:0) yielded thetitle compound as white solid (0.01 g, 16 %). MS: mle = 506.7 [M+Hf?.

As the paragraph descriping shows that 24340-77-0 is playing an increasingly important role.

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BISSANTZ, Caterina; BONNAFOUS, Rene; BUETTELMANN, Bernd; JAKOB-ROETNE, Roland; LERNER, Christian; RUDOLPH, Markus; WO2014/102233; (2014); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4576-90-3,Isothiazole-3-carboxylic acid,as a common compound, the synthetic route is as follows.

To a suspension of isothiazole-3-carboxylic acid (2 g, 15.49 mmol) in DCM at 0 C was added oxalyl dichloride (1.3 equiv.) followed by three drops of DMF. Bubbling commenced, and the reaction was warmed to 23 C after 10 min. The mixture was stirred for 3 h, then cooled to 0 C. N,0-dimethylhydroxylamine hydrochloride (1.3 equiv.) was added to the reaction, followed by triethylamine (3.5 equiv.) which was added dropwise via syringe over 10 min. Reactions was warm slowly to 23 C overnight, and stirred for a total of 15 h. Reaction mixture was diluted with IN HC1 solution and dichloromethane (1 :1 ratio). Layers were separated, and the aqueous layer was extracted with DCM (2x). Combined organic layers were dried over magnesium sulfate, filtered, and the solvent was removed in vacuo. Crude reside purified via silica gel chromatography (utilizing a hexane/ethyl acetate mix as eluent) to deliver the desired intermediate, N-methoxy-N-methylisothiazole-3-carboxamide (1 g, 38%> yield) as a pale yellow solid. NMR (400 MHz, CDCI3) delta ppm 8.67 (d, 1 H), 7.69 (br s, 1 H), 3.80 (s, 3 H), 3.46 (br s, 3 H).

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Reference£º
Patent; IRONWOOD PHARMACEUTICALS, INC.; BARDEN, Timothy Claude; SHEPPECK, James Edward; RENNIE, Glen Robert; RENHOWE, Paul Allan; PERL, Nicholas; NAKAI, Takashi; MERMERIAN, Ara; LEE, Thomas Wai-Ho; JUNG, Joon; JIA, James; IYER, Karthik; IYENGAR, Rajesh R.; IM, G-Yoon Jamie; (293 pag.)WO2016/44447; (2016); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com