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
Example 5Preparation of 5-[2-[4-(l,2-benzisothiazol-3-yl)-l-piperazinyn]ethyl]-6- chloro-l,3-di hydro-2H- indol-2-one:Charge 1.0 litre water, 100 gm of 5-(2-chloroethvl)-6-chlorooxindole product, 122.4 gm 3-(l-piperazinyl)-l,2-benzisothiazole HCI and 138.2 gm of sodium carbonate into a 3 litre three neck flask at 25 to 30 C. Stir for 15 minutes and heat to reflux temperature 95 to 100 C. Maintain at reflux temperature for 15 hrs. Cool the reaction mixture to 45 – 50C. Add 1.0 It of water into the reaction mixture and stir for 30 minutes. Filter at 45 to 50 C and wash with water. Suck dry for 30 minutes to yield crude product. Charge 2 It of water and above crude product and heat the mixture gradually to 45 to 50C and stir for 30 minutes. Filler the product at 45 to 50C and wash with water. Suck dry the product for 30 minutes. Charge 2.0 It of water and 300 gm of crude product into a 1.0 litre three neck flask at 25 to 30C and heat the mixture gradually to 45 to 50C. Stir for 30 mins. Filter the product at 45 to 50C and wash with water till about neutral pH (6.5 to 7.0). Suck dry the product for 30 minutes to get wet crude base 5-[2-[4-(l,2-benzisothiazo.-3-yl)-l-piperazinyl]ethylj-6- chloro-i,3-di hydro- 2H- indol-2-one. Add 300.-gms of wet crude base and 1.0 It of isopropanol at 25 to 30C. Warm the reaction mixture to 50 to 55C and stir for 1.0 hr. Cool the reaction mixture gradually to 10 to 15C and stir for 30 mins. Filter the product and wash with chilled isopropanol. Suck dry for 30 minutes. Charge 300gm of wet crude base and 6 It of tetrahydrofuran (THF). Heat the reaction mixture gradually to reflux temperature 65-70C. Reflux till clear solution. Cool to 50 to 55C and add charcoal and stir for 30 min at 50 to 55dC. Filter the charcoal and wash with hot THF. Distill out THF at 50 to 55 C under vacuum till residual volume is 1 It and cool the reaction mixture gradually to 5 to 10C and stir for 1 hr. Filter the product and wash with chilled THF. Suck dry the product for 30 minutes. Dry the product at 60 to 65C.
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Reference£º
Patent; ARCH PHARMALABS LIMITED; GHOGARE, Bhausaheb Nana; DESHPANDE, Uday K.; PAI, Ganesh Gurpur; MANDAL, Arun Kanti; CHARANJIT, Sehgal; NEHA, Dixit Akshaya; WO2012/20424; (2012); A1;,
Isothiazole – Wikipedia
Isothiazole – ScienceDirect.com