Category: 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

EXAMPLE 3 3-(1-Piperazinyl)-1,2-benzisothiazole¡¤hydrochloride Anhydrous piperazine (49.4 g, 0.57 mol) and t-butanol (10 mL) were added to a dry, 300 mL round bottom flask equipped with a mechanical stirrer, thermometer, condenser topped with a nitrogen inlet, and pressure-equalizing dropping funnel. After the flask was purged with nitrogen, it was heated to 100 C. in an oil bath. A solution of 3-chloro-1,2-benzisothiazole (19.45 g, 0.11 mol) in t-butanol (10 mL) was added to the addition, funnel, and then slowly added to the reaction flask over 20 minutes to moderate an exothermic reaction (112-118 C.). Once addition was complete the yellow solution was heated to reflux (121 C.) and then maintained at reflux for 24 hours. Thin-layer chromatography showed that the reaction was complete. The reaction mixture was cooled to 85 C. and 120 mL of water was added. The hazy solution was filtered and the filter cake rinsed with 60 mL of t-butanol/water (1:1) solution. The pH of the combined filtrate and wash was adjusted to 12.2 with 50% aqueous caustic. The aqueous solution was extracted with toluene (200 mL), the layers were separated, and the aqueous layer was extracted with fresh toluene (100 mL). The combined toluene layers were washed with water (75 mL), and then the toluene solution was concentrated in vacuo at 48 C. to 90 mL. Isopropanl (210 mL) was added to the concentrate and then the pH was slowly adjusted to 3.8 with 7.6 mL of concentrated hydrochloric acid. The resulting slurry was cooled to 0 C., granulated for 45 min, and then filtered. The filter cake was washed with cold isopropanol (50 mL) and then dried in vacuo at 40 C. to afford 23.59 g (80% yield) of 3-(1-piperazinyl)-1,2-benzisothiazole hydrochloride as an off white solid.

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

Reference£º
Patent; Pfizer, Inc.; US6111105; (2000); 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.

Preparation 1 SYNTHESIS OF 3-PIPERAZIN-1-YLBENZO[D]ISOTHIAZOLE A mixture of anhydrous piperazine (2.75 g, 32 mmol) and 3-chlorobenzo[d]isothiazole (1.00 g, 5.80 mmol) were heated in a sealed tube in an oil bath at 125¡ã C. for 24 hours. The orange melt was then quenched with ice water and 50percent NaOH was added in one portion. The mixture was extracted with dichloromethane to get the crude product which was purified by recrystallization to afford the title compound as a pale yellow solid in 24percent yield (0.260 g). MS (ES+) m/z 220 (M+1).

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

Reference£º
Patent; XENON PHARMACEUTICALS INC.; US2008/125434; (2008); 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.7716-66-7,3-Chlorobenzo[d]isothiazole,as a common compound, the synthetic route is as follows.

(a) 3-(1-PIPERAZINYL)-1,2-BENZOISOTHIAZOLE STR50 A mixture of 3-chloro-1,2-benzisothiazole (37.8 g., 0.235 mole) and piperazine (304.2 g., 3.53 mole) is heated under an argon atmosphere for a period of 20 hr. at 120 C. in a closed reactor. The reaction mixture is dissolved in 2 liters of water and the aqueous solution repeatedly extracted with methylene chloride. Extracts are combined, dried over magnesium sulfate and concentrated in vacuo. Residual material is taken up in ether, filtered and concentrated in vacuo to afford 24.4 g. (47%) of 3-(1-piperazinyl)-1,2-benzisothiazole free base as a viscous oil. A sample of the free base converted to the hydrochloride salt in ether with ethanolic hydrogen chloride and crystallized from methanol-ethanol affords analytically pure 3-(1-piperazinyl)-1,2-benzisothiazole hydrochloride, m.p. 280 C. (dec.). Anal. Calcd. for C11 H13 N3 S.HCl: C, 51.66; H, 5.52; N, 16.43. Found: C, 51.34; H, 5.46; N, 16.16.

7716-66-7 3-Chlorobenzo[d]isothiazole 598190, aisothiazole compound, is more and more widely used in various.

Reference£º
Patent; Mead Johnson & Company; US4487773; (1984); A;,
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

EXAMPLE 1 3-(1-Piperazinyl)-1,2-benzisothiazole STR26 A mixture of 3-chloro-1,2-benzisothiazole (37.8 g., 0.235 mole) and piperazine (304.2 g., 3.53 mole) is heated under an argon atmosphere for a period of 20 hr. at 120 C. in a closed reactor. The reaction mixture is dissolved in 2 liters of water and the aqueous solution repeatedly extracted with methylene chloride. Extracts are combined, dried over magnesium sulfate and concentrated in vacuo. Residual material is taken up in ether, filtered and concentrated in vacuo to afford 24.4 g. (47%) of 3-(1-piperazinyl)-1,2-benzisothiazole free base as a viscous oil. A sample of the free base converted to the hydrochloride salt in ether with ethanolic hydrogen chloride and crytallized from methanol-ethanol affords analytically pure 3-(1-piperazinyl)-1,2-benzisothiazole hydrochloride, m.p. 280 C. (dec.). Anal. Calcd. for C11 H13 N3 S.HCl: C, 51.66; H, 5.52; N, 16.43. Found: C, 51.34; H, 5.46; N, 16.16.

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

Reference£º
Patent; Mead Johnson & Company; US4411901; (1983); 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.

A solution of 3-(4-(4-fluorophenyl)-1-piperidyl)-1-propanol (10 g) in dry toluene (150 ml) was treated portionwise with a 50percent xylene suspension of sodium hydride (3 g). A solution of 3-chloro-1,2-benzisothiazole (3.6 g) in dry toluene (30 ml) was added dropwise at room temperature followed by stirring for 1.5 h at room temperature. Ice was added, the phases separated and the aqueous phase extracted with ether. Drying of the combined organic phases over magnesium sulfate and removal of solvents in vacuo gave an oil which was applied to column chromatography (silica gel, eluent:ethyl acetate/heptane/triethyl amine=50:50:4). The title compound 21 crystallized from a mixture of isopropyl ether/heptane. Yield: 1.5 g, mp: 91¡ã-92¡ã C.

7716-66-7 3-Chlorobenzo[d]isothiazole 598190, aisothiazole compound, is more and more widely used in various.

Reference£º
Patent; Lundbeck; H.; US5665725; (1997); A;,
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

3-Chlorobenzo[d]isothia-zole (300 mg, 3.0 mmol) was dissolved in propane- 1,3 -diamine (3 mL) and heated at 8O0C for 3 h. The reaction mixture was cooled to room temperature, poured into water and extracted with ethyl acetate. The organic extract was dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure to yield ^-(benzotdJisothiazol-S-ytypropane- 1,3-diamine as a yellow solid, (530 mg). 1H NMR (300 MHz, CDCl3): 7.8 (m, IH), 7.7 (m, IH), 7.5 (m, 2H), 7.3 (m, IH), 3.7 (m, 2H), 2.9 (t, 2H), 1.9 ppm (m, 2H).

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

Reference£º
Patent; RIGEL PHARMACEUTICALS, INC.; WO2006/91858; (2006); 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

(a) A mixture of 32 parts of ethyl 1-piperazinecarboxylate, 17 parts of 3-chloro-1,2-benzisothiazole and 45 parts of N,N-dimethylacetamide was stirred for 0.5 hours at 150¡ã C. After cooling to 50¡ã C., the reaction mixture was poured into ice water. The aqueous layer was decanted and the oily layer was stirred in water. The product from the oil layer was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 13 parts (44percent) of ethyl 4-(1,2-benzisothiazol-3-yl)-1-piperazinecarboxylate as a residue (int. 3).

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

Reference£º
Patent; Janssen Pharmaceutica N.V.; US4957916; (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.

Ethylenediamine (45 mL) was heated to 80 0C. A room temperature solution of 3-chlorobenzo[d]isothiazole (12g, 70.7 mmol) in ethylenediamine (5 mL) was added to the heated ethylenediamine dropwise. The resulting solution was heated at 80 0C for 3 h. The reaction mixture was cooled to room temperature and water (75 mL) was added. The aqueous mixture was extracted with ethyl acetate twice and the ethyl acetate layers were separated. The combined organic layers were dried over anhydrous sodium sulfate, filtered and the filtrate concentrated under reduced pressure to yield N1-(benzo[d]isothiazol-3-yl)ethane-l,2-diamine as a light yellow solid (8 g). 1H-NMR (300 MHz, CDCl3): 7.79-7.64 (m, 2H), 7.52 (t, IH), 7.34 (t, IH), 5.60 (broad s, IH), 3.62 (t, 2H), 3.08 ppm (t, 2H).

7716-66-7 3-Chlorobenzo[d]isothiazole 598190, aisothiazole compound, is more and more widely used in various.

Reference£º
Patent; RIGEL PHARMACEUTICALS, INC.; WO2006/91858; (2006); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com