Day: September 22, 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

N-[4-(2-BROMO-ETHYL)-2-FLUORO-PHENYL]-ACETAMIDE (0.2609 g, 1.00 mmol), 3-piperazin-1-yl-benzo [AGISOTHIAZOLE HYDROCHLORIDE (0.3887 g, 1.52 mmol), potassium carbonate (0.2109 g, 1.53 mmol), potassium iodide (0.1662 g, 1.00 MMOL) and acetonitrile (5.0 mL) were added to a Smith microwave reaction tube containing a magnetic stir bar and then crimped shut. The reaction was run on a Smith Personal Chemistry microwave at 140 C for 0.5 h. After removing the crimped septum, the contents were transferred to a separatory funnel with water (10 mL) and extracted with methylene chloride (2 x 40 mL). The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated to give an oily residue. Purification by MPLC on a 40M silica gel cartridge using a linear gradient over 1 h of 0-3% methanol in methylene chloride provided 0.1230 g (0.309 MMOL) of the product as an off-white solid after drying in vacuo. Several fractions containing product and a by-product (0.1487 g total) were discarded. Yield : 31% ; MS (APCI) : 399.2 [M+H] + ; Anal. Calcd. For C2IH23FN40S’0. 25 H20 : C, 62.59 ; H, 5.88 ; N, 13.90. Found: C, 62.72 ; H, 5.53 ; N, 13.53.

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

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

2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide, cas is 936-16-3, it is a common heterocyclic compound, the isothiazole compound, its synthesis route is as follows.,936-16-3

To a solution of {1-(tert-butyl)-5-(4-piperidin-1-yl-phenyl)-1H-pyrazol-3-yl}methanol (54.9 mg, 0.175 mmol) in methylene chloride (1.5 mL) were added PPh3 (93.1 mg, 0.355 mmol) and CBr4 (121 mg, 0.365 mmol) at 0¡ã C., followed by stirring at the same temperature for one hour to give {1-(tert-butyl)-5-(4-piperidin-1-yl-phenyl)-1H-pyrazol-3-yl}methyl bromide. When the reaction was completed as measured by TLC(Hexane:EtOAc=2:1), 1,2-benzisothiazoline-1,1-dioxide (27.3 mg, 0.161 mmol) in N,N-dimethylformamide (1.5 mL) was added dropwise. At the same temperature, potassium carbonate (228 mg, 1.65 mmol) was added, and the resulting solution was stirred for a day. When the reaction was completed as measured by TLC (Hexane:EtOAc=2:1), water was added, after which extraction was carried out with ethyl acetate and brine. The organic layer thus formed was dried over anhydrous magnesium sulfate, and concentrated in vacuo. The concentrate was purified by column chromatography (Hexane:EtOAc=4:1?1:1) to afford the title compound (15.2 mg, 20percent, white solid). (0324) M.P. 150.4-165.2¡ã C.; (0325) 1H NMR (300 MHz, CDCl3) delta 7.89 (d, J=7.9 Hz, 1H), 7.64-7.52 (m, 2H), 7.40 (d, J=7.1 Hz, 1H), 7.30-7.17 (m, 2H), 6.29 (d, J=8.7 Hz, 2H), 6.22 (s, 1H), 4.52 (s, 2H), 4.46 (s, 2H), 3.26-3.23 (brs, 4H), 1.79-1.74 (brs, 4H), 1.67-1.63 (brs, 2H), 1.49 (s, 9H); (0326) 13C NMR (75 MHz, CDCl3) delta 151.9, 144.4, 143.3, 135.4, 134.3, 132.5, 131.1, 128.9, 124.5, 123.7, 121.4, 114.9, 109.0, 61.0, 50.0, 41.4, 31.2, 25.7, 24.3

As the rapid development of chemical substances, we look forward to future research findings about 936-16-3

Reference£º
Patent; KOREA INSTITUTE OF SCIENCE AND TECHNOLOGY; NAM, Ghil Soo; CHOI, Kyung Il; KIM, Jung Hyun; PAE, Ae Nim; HONG, Jin Ri; LEE, Jae Kyun; (30 pag.)US2015/329533; (2015); 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.936-16-3,2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide,as a common compound, the synthetic route is as follows.

936-16-3, Step 2. A mixture of 14 (200 mg, 0.70 mmol), 1 (143 mg, 0.84 mmol), Cs2CO3 (459 mg, 1.41 mmol), Cul (40 mg, 0.21 mmol) and 2-(dimethylamino)acetic acid hydrochloride (30 mg, 0.21 mmol) in dioxane (2 mL) was degassed and purged with N2 (3X). The mixture was stirred at 100¡ãC for 12 h under N2 atmosphere. The reaction mixture was diluted with ethyl acetate (50 mL), adjusted to pH=7 with 2N HC1, and separated. The aqueous layer was extracted with ethyl acetate (2 x 40 mL) and the combined organic layer was washed with saturated brine (80 mL), dried over anhydrous sodium sulfate, filtered and concentrated to give 15 (230 mg) as a light yellow solid.

As the paragraph descriping shows that 936-16-3 is playing an increasingly important role.

Reference£º
Patent; NUMERATE, INC.; RAIMUNDO, Brian; KOLTUN, Elena S.; GRIFFIN, John; STANGELAND, Eric; (93 pag.)WO2018/49324; (2018); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com

7716-66-7, 3-Chlorobenzo[d]isothiazole is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

7716-66-7, General procedure for synthesis of 3-(piperazin-1-yl)benzo[d]isothiazole The compound 3-chloro-1, 2-benzisothiazole (1 mmol) was allowed to react with piperazine (1.2 mmol) in Ethanol at 80 ¡ãC for 36 h. Then reaction mixture was concentrate and RM was dissolved in ethyl acetate and washed with water. Ethylacetate layer dried with Na2SO4 and concentrate them and get 3-(piperazin-1-yl)benzo[d]isothiazole. White solid, 85percent yield, mp 215-217 ¡ãC, 1H NMR (400 MHz, CDCl3): delta = 7.42 (t, J = 7.2 Hz, 1H), 7.29 (m, 3H), 4.14 (t, J = 4.8 Hz, 4H), 3.15 (t, J = 4.8 Hz, 4H); 13C NMR (100 MHz, DMSO+CDCl3): 166.8, 156.2, 135.8, 128.5, 127.6, 125.2, 124.9, 119.8, 53.6, 49.2, 46.6, 45.1, 7.1. MS calcd for C19H20N4OS2: 219.31. Found: 220.33, (M+); Anal. Calcd for C19H20N4OS2: C, 60.24; H, 5.97; N, 19.16; S, 14.62; Found: C, 60.25; H, 5.99; N, 19.13; S, 14.61.

As the paragraph descriping shows that 7716-66-7 is playing an increasingly important role.

Reference£º
Article; Reddy, Kummetha Indrasena; Srihari, Konduri; Renuka, Janupally; Sree, Komanduri Shruthi; Chuppala, Aruna; Jeankumar, Variam Ullas; Sridevi, Jonnalagadda Padma; Babu, Kondra Sudhakar; Yogeeswari, Perumal; Sriram, Dharmarajan; Bioorganic and Medicinal Chemistry; vol. 22; 23; (2014); p. 6552 – 6563;,
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

8. Preparation of ZPR in glycerol by Na C03 portion-wise addition To a three necked flask was charged BITP HC1 (15g), CEI (16. 2g), glycerol (60ml) and Na2C03 (3. 11 g, 0. 5mol). The reaction mixture was heated at 115 C and after 15′ a new portion of 0.12 mol Na2C03 was added. The heating was continued by addition of 0.12 mol base each hour. After 5 hours the base addition was completed and the reaction mixture was heated for an additional hour. After cooling to room temperature, the mixture was diluted with water (120ml) and after 1 hour stirring the product crude was filtrated, washed with water and dried at 50C to afford 25.7g dried product (yield 82. 4%) (purity by HPLC 94%).

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.936-16-3,2,3-Dihydrobenzo[d]isothiazole 1,1-dioxide,as a common compound, the synthetic route is as follows.,936-16-3

Example 89 2-[{1-(tert-Butyl)-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl}methyl]-2,3-dihydro[d]isothiazole 1,1-dioxide (Compound 34) To a solution of 1,2-benzisothiazoline-1,1-dioxide (24.3 mg, 0.144 mmol) in N,N-dimethylformamide (1 mL) was added dropwise potassium carbonate (180 mg, 1.30 mmol) at room temperature, followed by stirring for 15 min. This solution was slowly added with drops of {1-(tert-butyl)-5-(4-trifluoromethylphenyl)-1H-pyrazol-3-yl}methyl bromide (51.6 mg, 0.143 mmol) in methylene chloride (4.5 mL), and stirred for a day at room temperature. When the reaction was completed as measured by TLC (Hexane:EtOAc=4:1), the reaction mixture was filtered through celite. The filtrate was neutralized with 1M HCl and an aqueous saturate sodium hydrogen carbonate solution. After extraction with ethyl acetate and water, the organic layer thus formed was dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The concentrate was purified by column chromatography (Hexane:EtOAc=4:1?2:1) to afford the title compound (25.4 mg, 39percent, white solid). M.P. 144.6-148.2¡ã C.; 1H NMR (300 MHz, CDCl3) delta 7.85 (d, J=7.7 Hz, 1H), 7.68-7.48 (m, 6H), 7.41 (d, J=7.4 Hz, 1H), 6.29 (s, 1H), 4.54 (s, 2H), 4.47 (s, 2H), 1.49 (s, 9H); 13C NMR (75 MHz, CDCl3) delta 143.9, 142.4, 137.9, 135.3, 134.2, 132.6, 130.9, 130.8, 130.5, 129.0, 125.7, 124.8, 124.7, 124.5, 122.1, 121.5, 109.4, 61.5, 50.1, 41.3, 31.3

The synthetic route of 936-16-3 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; KOREA INSTITUTE OF SCIENCE AND TECHNOLOGY; NAM, Ghil Soo; CHOI, Kyung Il; KIM, Jung Hyun; PAE, Ae Nim; HONG, Jin Ri; LEE, Jae Kyun; (30 pag.)US2015/329533; (2015); 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

EXAMPLE 75 3-[4-[1-(1,2-Benzisothiazol-3-yl)-4-piperazinyl]-butyl]-1-thia-3-azaspiro[4.4]nonan-4-one A mixture of 3-(4-bromobutyl)-1-thia-3-azaspiro[4.4]-nonan-4-one (4.50 g), 1-(1,2-benzisothiazol-3-yl)piperazine hydrochloride (4.33 g), K2 CO3 (7.45 g) and NaI (560 mg), in acetonitrile (220 ml) was heated at 65 C. for 14.5 hours and the product was processed in substantially the same manner as in Example 10 to afford 2.25 g of crystals, m.p. 200-203 C. ANALYSIS: Calculated for C22 H30 N4 OS2 *HCl: 56.57%C; 6.69%H; 11.99%N; 7.59%Cl. Found: 56.15%C; 6.75%H; 12.11%N; 7.88%Cl.

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

Reference£º
Patent; Hoechst-Roussel Pharmaceuticals Inc.; US4933453; (1990); 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.7716-66-7,3-Chlorobenzo[d]isothiazole,as a common compound, the synthetic route is as follows.

7716-66-7, 3-Chloro-1 ,2-benzisothiazole (147 mg, 0.87 mmol) was added to a solution of the piperidine of preparation 60 (200 mg, 0.72 mmol) in acetonitrile (20 mi). 1 ,8-Diazabicyclo[5.4.0]undec-7-ene (111 mul, 0.72 mmol) was added, and the reaction mixture was then stirred at room temperature for 48 hours. It was then concentrated under reduced pressure and the crude product was purified by EPO column chromatography on silica gel using dichloromethane/methanol/aqueous ammonia as eluant (90:10:1 v/v/v) to yield the title compound (290 mg, 98percent) as a solid.1H NMR (400MHz, CD3OD): delta 1.80-1.85 (m, 2H), 2.00-2.10 (m, 2H), 2.23 (s, 3H), 2.57 (m, 1 H), 2.85-2.91 (m, 2H), 3.23-3.28 (m, 2H), 7.32 (t, 1 H), 7.43 (d, 2H), 7.61-7.68 (m, 4H), 7.74 (d, 1 H); LRMS APCI+ m/z 410 [MH]+.

The synthetic route of 7716-66-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; PFIZER LIMITED; WO2006/114706; (2006); 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.87691-88-1,3-Piperazinobenzisothiazole hydrochloride,as a common compound, the synthetic route is as follows.

87691-88-1, N-[4-(2-BROMO-ETHYL)-2-FLUORO-PHENYL]-ACETAMIDE (0.2609 g, 1.00 mmol), 3-piperazin-1-yl-benzo [AGISOTHIAZOLE HYDROCHLORIDE (0.3887 g, 1.52 mmol), potassium carbonate (0.2109 g, 1.53 mmol), potassium iodide (0.1662 g, 1.00 MMOL) and acetonitrile (5.0 mL) were added to a Smith microwave reaction tube containing a magnetic stir bar and then crimped shut. The reaction was run on a Smith Personal Chemistry microwave at 140 C for 0.5 h. After removing the crimped septum, the contents were transferred to a separatory funnel with water (10 mL) and extracted with methylene chloride (2 x 40 mL). The combined organic extracts were dried over anhydrous sodium sulfate, filtered and concentrated to give an oily residue. Purification by MPLC on a 40M silica gel cartridge using a linear gradient over 1 h of 0-3% methanol in methylene chloride provided 0.1230 g (0.309 MMOL) of the product as an off-white solid after drying in vacuo. Several fractions containing product and a by-product (0.1487 g total) were discarded. Yield : 31% ; MS (APCI) : 399.2 [M+H] + ; Anal. Calcd. For C2IH23FN40S’0. 25 H20 : C, 62.59 ; H, 5.88 ; N, 13.90. Found: C, 62.72 ; H, 5.53 ; N, 13.53.

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

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

7716-66-7,7716-66-7, 3-Chlorobenzo[d]isothiazole is a isothiazole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Piperazine (508.8 g) and Tert. Butanol (200 ml) were placed in round bottom flask (RBF) and then the resulting solution heated up to 90 to 100 degree C. 3-chloro-1,2-benzisothiozole (40 g) was added to the solution 5 times with in time interval of 5 to 20 minutes at the same temperature. Temperature was raised up to 110 to 130 degree C. and maintained for 16 hours. After confirmation of the completion of the reaction by TLS (Thin Layer Chromatography), the resulting solution was cooled to 80 to 90 degree C. followed by addition of water (800 ml). The above mixture was cooled to 25 to 35 degree C. and was filtered to remove the solid particles. Water (100 ml) was added to the filtrate and then pH was raised to 12-14 with caustic lye (75 ml). Toluene (400 ml) was added to the alkaline solution the resulting bi-phasic mixture was stirred vigorously for 15 to 30 minutes at 25 to 35 degree C. Organic layer separated and the aqueous layer was multiply extracted with toluene followed by combing all organic layers. The combined organic layer was washed with water (200 ml). Active carbon (10 g) was added to the washed organic layer and then filtered out the carbon. The organic solvent was evaporated till the volume reaches to 150 to 200 ml. The resulting concentrated solution was cooled to 0 to 5 degree C. and maintained for about 2 hours. Separated solids were filtered and then washed with chilled toluene (20 ml). Finally, Isolated compound was dried under reduced pressure to get titled compound 130 to 135 g.

The synthetic route of 7716-66-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; DR. REDDY’S LABORATORIES LIMITED; DR. REDDY’S LABORATORIES, INC.; US2005/49295; (2005); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com