HRID1493269

反应详情

EQUATION

反应方程式

HRID 1493269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

The experiment is carried out as in Example 1, starting with 2(3-chloropropyl)naphtho[1,8-cd]isothiazole 1,1-dioxide(8.4 g), triethylamine (4.2 cc) and 4-(3-fluorophenyl)piperazine (5.3 g) in toluene (100 cc). The mixture is heated for 8 hours at boiling point, then cooled to a temperature of about 20° C. After purification by flash-chromatography on a silica column, under a current of argon at medium pressure (0.5-1.5 bar) with dichloromethane and then a mixture of dichloromethane and ethyl acetate (5-50 vol) as eluant, and recrystallization from boiling acetonitrile (20 cc), 2-(3-[4-(3-fluorophenyl)-1-piperazinyl]propyl}naphtho[1,8cd]isothiazole 1,1-dioxide (4.7 g) is obtained, m.p. 103° C.

WORKUP

后处理

  1. temperatureThe mixture is heated for 8 hours
  2. customAfter purification by flash-chromatography on a silica column
  3. additionunder a current of argon at medium pressure (0.5-1.5 bar) with dichloromethane and then a mixture of dichloromethane and ethyl acetate (5-50 vol) as eluant
  4. customrecrystallization