反応 #7691

反応方程式

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

溶媒

isopropanol

反応条件

後処理

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

実験手順

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.

出典