반응 #7691

반응 방정식

hydrogen chloride

5-(2-(4-(1,2-benzisothiazol-3-yl)-1-piperazinyl)ethyl)-6-chloro-1,3-dihydro-2H-indol-2-one

methyl isobutyl ketone

→

5-[2-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]ethyl]-6-chloro-1, 3-dihydro-2H-indol-2-one hydrochloride

용매

isopropanol

반응 조건

후처리

1. 1
   기타To a flask equipped with magnetic stirrer
2. 2
   workup.STIRRINGthe mixture was stirred for about 24 h
3. 3
   여과The product was collected by filtration on a Buchner funnel
4. 4
   세척The filter cake is rinsed with 3×10 mL of methyl isobutyl ketone at 20–25° C.
5. 5
   기타transferred to a drying oven
6. 6
   기타dried in vacuo at 65–70° C. for about 24 h

실험 절차

To a flask equipped with magnetic stirrer, thermometer and nitrogen inlet was added 5-(2-(4-(1,2-benzisothiazol-3-yl)-1-piperazinyl)ethyl)-6-chloro-1,3-dihydro-2H-indol-2-one free base (5.0 g) and methyl isobutyl ketone (100 mL) and the suspension was stirred at 20–25° C. under nitrogen. A 20.5% anhydrous solution of hydrogen chloride in isopropanol (6.45 g) was added and the mixture was stirred for about 24 h. The product was collected by filtration on a Buchner funnel. The filter cake is rinsed with 3×10 mL of methyl isobutyl ketone at 20–25° C. and transferred to a drying oven and dried in vacuo at 65–70° C. for about 24 h. This afforded 5.25 g of anhydrous ziprasidone hydrochloride. The material contained 0.52% of residual methyl isobutyl ketone, as determined by NMR.

출처