反应 #320404

反应方程式

6-fluoro-3-(4-piperidinyl)-1,2-benzisothiazole

ethyl 3-bromopropionate

K2CO3

HCl

→

desired compound

收率 64.0%

Ethyl 3-[4-(6-Fluoro-1,2-benzisothiazol-3-yl)-1-piperidinyl]propionate hydrochloride

收率 64.0%

溶剂

Et2O

CH3CN

EtOAc

H2O

反应条件

后处理

1. 1
   温度refluxed for 16 hours
2. 2
   其他to precipitate 6.3 g of a white hydrochloride salt
3. 3
   其他The salt was recrystallized from CH3CN

实验过程

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisothiazole (6.0 g, 25 mmol), ethyl 3-bromopropionate (4.5 g, 25 mmol), K2CO3 (3.5 g) and CH3CN (100 ml) was stirred and refluxed for 16 hours. The reaction was poured into H2O, and after extractive workup with EtOAc, 6.0 g of an orange oil was realized. The oil was dissolved in Et2O and ethereal HCl was added to precipitate 6.3 g of a white hydrochloride salt. The salt was recrystallized from CH3CN to yield 6.0 g (64%) of the desired compound. An analytical sample was obtained by recrystallization of a 1.0 g sample from EtOH-Et2O to yield 0.8 g of a white solid, m.p.=197°-199° C.

来源