反应 #83926

反应方程式

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

1-[4-(3-chloropropoxy)-3-hydroxyphenyl]ethanone

NaHCO3

CH3CN

→

dark solid

收率 97.0%

1-[4-[3-[4-(6-Fluoro-1,2-benzisothiazol-3-yl)-1-piperidinyl]propoxy]-3-hydroxyphenyl]ethanone

收率 97.0%

溶剂

H2O

反应条件

后处理

1. 1
   温度at reflux under N2 for 65 hours
2. 2
   其他The cooled reaction
3. 3
   萃取the aqueous mixture was extracted with EtOAc
4. 4
   萃取The EtOAc extract
5. 5
   洗涤was washed with H2O (1×) and brine (3×)
6. 6
   干燥after drying with MgSO4 the solvent
7. 7
   其他was evaporated

实验过程

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisothiazole (2.4 g, 10.1 mmol), 1-[4-(3-chloropropoxy)-3-hydroxyphenyl]ethanone (2.5 g, 11.1 mmol), NaHCO3, (0.94 g, 11.1 mmol), KI (100 mg) and CH3CN (100 ml) was stirred at reflux under N2 for 65 hours. The cooled reaction was poured into H2O and the aqueous mixture was extracted with EtOAc. The EtOAc extract was washed with H2O (1×) and brine (3×) and after drying with MgSO4 the solvent was evaporated to give 4.2 g of a dark solid. Three consecutive recrystallizations from EtOH provided 2.1 g (48%) of glittery beige crystals m.p.=135°-137° C.

来源