Month: October 2020

3-Piperazinobenzisothiazole hydrochloride, cas is 87691-88-1, it is a common heterocyclic compound, the isothiazole compound, its synthesis route is as follows.,87691-88-1

To a solution containing 3- (1-piperazinyl) -1,2_ benzisothiazole hydrochloride (100g) and potassium carbonate (136g) in acetonitrile(800ml) was added a solution of 1-chloro-4-bromo-butane (88g). Vigorous stirring mixture was refluxed for 10 hours, the solvent was distilled off pressure acetonitrile was added water (100ml) and toluene (300ml) to the reaction mixture was distilled net was effected under stirring to break up the product mixture, refluxing under stirring operation , the net after the water addition, cooling down, the suspension was filtered to give a white inorganic salts and organic salts of a mixture of the crude quaternary spiro ammonium base (267g).

As the rapid development of chemical substances, we look forward to future research findings about 87691-88-1

Reference£º
Patent; Yantai Besten Pharmaceutical Co., Ltd.; Bi, Haidong; Zhang, Yifang; (8 pag.)CN105669665; (2016); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide, cas is 27148-03-4, it is a common heterocyclic compound, the isothiazole compound, its synthesis route is as follows.,27148-03-4

The complex was synthesized by addition of 4,4′-trimethylenedipyridine (6.2 mg, 0.031 mmol) and thiosaccharine (12.7 mg, 0.0638 mmol), respectively, to a solution of Zn(NO3)26H2O (10.2mg, 0.0342 mmol) in ethanol:water (4 ml), and kept under mechanical stirring at room temperature. The resulting yellow solid was filtered off and washed with cold water. By slow evaporation of the mother solution single crystals appeared. They were washed with water and analysed using X-ray diffraction. Yield: 82%. Molar conductivity (mS M1) = 28.3. Analytical percent composition calculated for C27H22N4O4S4Zn: C = 49.127%; H = 3.359%;N = 8.487%. Found: C = 48.811%; H = 2.981%; N = 8.378%. Soluble in DMSO and DMF. Slightly soluble in water, ethanol, methanol, chloroform. Insoluble in acetone and methane dichloride. UV-Visible [DMSO, kmax nm]: 347.1H NMR (300 MHz, DMSO) d 8.46 (dd, 4H), 7.92 (m, 2H), 7.58-7.72 (m, 6H), 7.28 (dd, 4H), 2.64 (t, 4H), 1.93 (m, 2H). 13C NMR (75 MHz, DMSO) d 191.71 (C1), 151.07 (C10), 149.31 (C8), 137.98(C7), 136.56 (C2), 132.05 (C4), 130.82 (C5), 125.07 (C3), 124.04(C9), 119.01 (C6), 33.80 (C11), 30.12 (C12).

As the rapid development of chemical substances, we look forward to future research findings about 27148-03-4

Reference£º
Article; Delgado, Fermin; Freire, Eleonora; Baggio, Ricardo; Gonzalez Pardo, Veronica; Dorn, Viviana; Dennehy, Mariana; Inorganica Chimica Acta; vol. 479; (2018); p. 266 – 274;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.76857-14-2,Sodium 3-oxido-5-sulfidoisothiazole-4-carboxylate,as a common compound, the synthetic route is as follows.,76857-14-2

The second intermediate obtained in step (4) is added in portions to the aqueous solution of 4-carboxy-3-hydroxy-5-mercaptoisothiazole trisodium in acetone at a low temperature of 2 to 8C.Then, the pH of the mixed solution was adjusted with sodium bicarbonate to be 7.5 to 9, and allowed to react at 15 to 30 C. and a stirring rate of 30 to 80 r/min for 3 to 8 hours.After filtering, the filter cake is washed with a small amount of deionized water to neutrality, and then dried under reduced pressure to obtain crude cefotetan acid; The cefotetan acid crude product obtained in step (5) is configured as an aqueous acetone suspension, and the excess sodium bicarbonate is stirred and dissolved in batch at room temperature.Then use activated carbon to stir for more than 1h, filter, -5 ~ 5 C,Stir and add 5 ~ 8mol/L hydrochloric acid solution to adjust the pH to less than 3, stir, filter and dry to obtain purified cefotetanic acid; The method for adding sodium bicarbonate is as follows: first, sodium bicarbonate is added in an amount of 30 to 50 g per batch, and after each batch is added,After stirring for 1-3 hours to dissolve, add the next batch, and so on, until the added sodium bicarbonate does not dissolve; At a low temperature of -5 to 10C, cefotetan obtained in step (6) is dissolved in purified water, and then sodium bicarbonate is added in portions.Stir and dissolve and adjust the pH of the solution to below 6, then add the activated carbon to stir for more than 1h, filter,The filtrate is first filtered through a 0.25 mum nylon filter and then filtered through a 0.2-0.3 mum filter.Finally, it is filtered through a nanofiltration membrane of 10 to 50 nm, then sterilized in a sterilization chamber, and freeze-dried at -40 C. to -15 C. for more than 12 hours to obtain the disodium cefotetan.

76857-14-2 Sodium 3-oxido-5-sulfidoisothiazole-4-carboxylate 136151974, aisothiazole compound, is more and more widely used in various fields.

Reference£º
Patent; Jiangsu Han Sitong Pharmaceutical Co., Ltd.; Wang Duoping; Wei Genghu; Shi Jiagui; Lu Lihuan; (9 pag.)CN107540694; (2018); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

27148-03-4, Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

A solution of thiosaccharin (tsacH) (0.084 g, 0.425 mmol) in chloroform (10 cm3) was added to a solution of [Pt(kappa2-dppm)2]Cl2 (0.22 g, 0.22 mmol) in chloroform (10 cm3). A few drops of triethylamine were added and the resulting mixture was heated under reflex for 1 h. This produced a yellow solution which was filtered and reduced to half volume. Methanol (2 cm3) was added and the mixture was set aside to evaporate slowly at room temperature. The pale yellow crystalline solid thus formed was filtered off and dried in a vacuum oven (85%). 11: pale yellow solid, 85% yield. 1H NMR: delta 7.57 (d, J 7.60 Hz, 4H, Ar), 7.50-6.80 (m, 44 H, Ar), 3.46 (br, 4H, CH2); 31P{1H} NMR: 253 K 18.1 (br), -30.4 (br) ppm; 298 K 16.8 (vbr), -28.1 (vbr) ppm; 333 K -23.3 (vbr) ppm; IR(KBr) 3053w, 2932w, 1431s, 1313vs, 1159vs, 994s, 800s, 694s, 378m cm-1; Elemental Anal. Calc. for PtN2S4P4O4C64H52¡¤0.5CH2Cl2. Found: C, 55.42 (55.00); H, 3.79 (3.66); N: 2.00 (1.97)%., 27148-03-4

The synthetic route of 27148-03-4 has been constantly updated, and we look forward to future research findings.

Reference£º
Article; Al-Jibori, Subhi A.; Al-Jibori, Mohamed H.S.; Hogarth, Graeme; Inorganica Chimica Acta; vol. 398; (2013); p. 117 – 123;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.87691-88-1,3-Piperazinobenzisothiazole hydrochloride,as a common compound, the synthetic route is as follows.

87691-88-1, To a solution containing 3- (1-piperazinyl) -1,2_ benzisothiazole hydrochloride (100g) and potassium carbonate (136g) in acetonitrile (800ml) added 1,4_ dibromobutane suspension ( 110g). Vigorous stirring mixture was refluxed for 10 hours, the solvent was distilled off pressure acetonitrile was added water (100ml) and toluene (300ml) to the reaction mixture was distilled net was effected under stirring to break up the product mixture, refluxing under stirring operation , the net after the water addition, cooling down, the suspension was filtered to give a white inorganic salts and organic salts of a mixture of the crude quaternary spiro ammonium base (280g).

87691-88-1 3-Piperazinobenzisothiazole hydrochloride 11521711, aisothiazole compound, is more and more widely used in various fields.

Reference£º
Patent; Yantai Besten Pharmaceutical Co., Ltd.; Bi, Haidong; Zhang, Yifang; (8 pag.)CN105669665; (2016); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

27148-03-4, Benzo[d]isothiazole-3(2H)-thione 1,1-dioxide is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a thf solution (20mL) of [Ru3(CO)12] (100mg, 0.16mmol) was added tsacH (63mg, 0.32mmol). The reaction mixture was heated to reflux for 4h, after which time the reaction mixture was then allowed to cool at room temperature. The solvent was removed under reduced pressure and the residue chromatographed by TLC on silica gel. Elution with n-hexane/CH2Cl2 (v/v, 1:1) developed four bands. The first band was unreacted [Ru3(CO)12] (14mg). The second band afforded [H2Ru3(CO)7(mu-N,S-tsac)(mu-C,N-C6H4CNSO2)(mu3-S)] (2) as orange crystals (24mg, 17%) after recrystallization from n-hexane/CH2Cl2 at 4C. The third band afforded two types of crystals (yellow and orange) after recrystallization from n-hexane/CH2Cl2 at 4C which were physically separated by hand. The orange crystals were characterized as [Ru2(CO)6(mu-N,S-tsac)2] (1) (7mg, 4%), while the yellow crystals were characterized as [Ru4(CO)12(mu-N,S-tsac)2(mu4-S)] (3) (10mg, 7%). The fourth band afforded [H2Ru5(CO)13(mu-N,S-tsac)(mu-C,N-C6H4CNSO2)(mu3-S)(mu4-S)] (4) (14mg, 11%) as orange crystals after recrystallization from n-hexane/CH2Cl2 at 4C. Data for 2: Anal. Calc. for C21H10N2O11Ru3S4: C, 28.10; H, 1.12; N, 3.12. Found: C, 28.32; H, 1.15, N, 3.14%. IR (nuCO, CH2Cl2): 2124vs, 2067vs, 2060sh, 2012s cm-1. 1H NMR (CDCl3): delta 8.29 (d, J 8.0Hz, 1H), 8.02 (m, 1H), 7.91 (t, J 7.2Hz, 1H), 7.85 (m, 1H), 7.82 (m, 1H), 7.78 (d, J 7.2Hz, 1H), 7.73 (m, 2H),-14.31 (d, J 0.8Hz, 1H),-16.14 (d, J 0.8Hz, 1H). Data for 3: Anal. Calc. for C26H8N2O16Ru4S5: C, 26.72; H, 0.69; N, 2.40. Found: C, 27.08; H, 0.74; N, 2.48%. IR (nuCO, CH2Cl2): 2124w, 2102s, 2087vs, 2066vs, 2021vs cm-1. 1H NMR (CD2Cl2): delta 8.06 (m, 1H), 7.99 (d, J 7.2Hz, 1H), 7.90-7.76 (m, 6H). Data for 4: Anal. Calc. for C27H10N2O17Ru5S5: C, 24.95; H, 0.78; N, 2.15. Found: C, 25.28; H, 0.85; N, 2.24%. IR (nuCO, CH2Cl2): 2124s, 2093s, 2066vs, 2041s, 2016s, 1958w cm-1. 1H NMR (CD2Cl2): aromatic region, major isomer, delta 8.13 (d, J 7.2Hz, 1H), 7.93-7.74 (m, 7H); hydride region, major isomer, delta-13.67 (d, J 2.0Hz, 1H),-15.55 (d, J 2.0Hz, 1H), minor isomer, delta-13.78 (d, J 2.0Hz, 1H),-16.07 (d, J 2.0Hz, 1H). Major/minor=21:1., 27148-03-4

Big data shows that 27148-03-4 is playing an increasingly important role.

Reference£º
Article; Mia, Md. Jadu; Reza, Md. Selim; Bhoumik, Nikhil C.; Ghosh, Shishir; Nesterov, Vladimir N.; Richmond, Michael G.; Kabir, Shariff E.; Journal of Organometallic Chemistry; vol. 906; (2020);,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.288-16-4,Isothiazole,as a common compound, the synthetic route is as follows.

To a solution of isothiazole (A.157) (3.0 g, 35.3 mmol) in 50 mL THF at -78 0C under argon was added n-butyllithium (1.6 M in hexane, 22.1 mL, 35.3 mmol) dropwise over 10 minutes. The mixture stirred at -780C for 1.5 hours. A solution of 2-fluoro-5-iodobenzaldehyde (A.156)(7.35 g, 29.4 mmol) in 30 mL THF was added dropwise over 15 minutes, and the reaction stirred an additional 2 hours at -78 0C. Water was added to quench the reaction, and the mixture warmed to 0 0C. The solution was neutralized with 2 N HCl to pH 7, partitioned between water and dichloromethane, and the aqueous layer further extracted with dichloromethane. The combined organic extracts were washed with brine, dried over MgSO4 and condensed. Purification by flash chromatography (0-15-100% ethyl acetate in hexane) gave 7.19 g (2- fluoro-5-iodophenyl)(isothiazol-5-yl)methanol A.158. IH NMR (500 MHz, CHLOROFORM- d) delta ppm 8.30 (1 H, s), 7.76 (1 H, dd, J=6.8, 2.2 Hz), 7.56 (1 H, ddd, J=8.6, 5.0, 2.3 Hz), 6.97 (1 H, s), 6.79 (1 H, dd, J=9.8, 8.8 Hz), 6.37 (1 H, s)

288-16-4, As the paragraph descriping shows that 288-16-4 is playing an increasingly important role.

Reference£º
Patent; AMGEN INC.; WO2009/158011; (2009); 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

87691-88-1, Excess dried, -325 mesh potassium carbonate (257 mg, 1.86 MMOL) was diluted in 4 mL acetonitrile and 3-piperazin-1-yl-benzoisothiazole hydrochloride (395 mg, 1.55 MMOL), catalytic potassium iodide, and 1 (2- chloroethoxy)-4-nitrobenzene (250 mg, 1.20 MMOL) were added. This mixture was sealed in a Smith microwave vial and heated on the Smith Workstation at 150 C for 1.5 h. After cooling, the salts were filtered off and washed with ACETONITRILE and the filtrate was concentrated. The residue was taken up in methylene chloride and washed with water. The organic layer was dried over sodium sulfate, and concentrated to afford 530 mg of a yellow solid. Yield 89%; 92% HPLC purity at 214 nm; mp 115 C ; MS (APCI) : 385 [M+H] +.

The synthetic route of 87691-88-1 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; WARNER-LAMBERT COMPANY LLC; WO2004/41793; (2004); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

18480-53-0, 3,4-Dichloroisothiazole-5-carboxylic acid is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

18480-53-0, EXAMPLE 5 Synthesis of isopropyl 3,4-dicloroisothiazole-5-carboxylate (Compound No. 6) Thionyl chloride (20 g) was added to 1.5 g of 3,4-dichloroisothiazole-5-carboxylic acid and the resultant mixture was heated under reflux for 1 hour. After excess thionyl chloride was distilled off under reduced pressure, a small amount of benzene was added, and the solvent was again distilled off under reduced pressure to remove a trace amount of thionyl chloride. Dry diethyl ether (10 ml) was added to the residue, whereby an acid chloride solution was obtained. 2-Propanol (0.54 g) and triethylamine (0.92 g) were dissolved in dry diethyl ether, to which the above-prepared acid chloride solution was added dropwise under ice cooling. They were then reacted at 30¡ã C. for 30 minutes and, after insoluble matter was filtered off, the filtrate was concentrated and then purified by chromatography on a silica gel column (n-hexane:ethyl acetate=9:1) to obtain 1.02 g of the title compound.

As the paragraph descriping shows that 18480-53-0 is playing an increasingly important role.

Reference£º
Patent; Mitsui Toatsu Chemicals, Incorporated; US5240951; (1993); A;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

936-16-3, 2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,936-16-3

General procedure: Potassium carbonate was dissolved in DMF, and 1,2-bezeneisothiazolin-1,1-dioxide (8) (1 equiv.) in dichloromethanewas added to the reaction solution, and stirred for overnight. Then,the reaction mixture was filtered through Celite, and washed with1 N HCl and saturated sodium hydrogen carbonate solution. Residualsolution was dried over magnesium sulfate, and concentratedin vacuo, and purified by column chromatography to afford the titlecompound.

936-16-3 2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide 13638, aisothiazole compound, is more and more widely used in various fields.

Reference£º
Article in Press; Hong, Jin Ri; Choi, Young Jin; Keum, Gyochang; Nam, Ghilsoo; Bioorganic and Medicinal Chemistry; (2017);,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com