HRID850723
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 35 °C
PROCEDURE
实验过程
Boron trichloride gas is condensed into a cold graduated cylinder (2.8 ml), and added to a solution of [6-methoxy-2-(4-methoxyphenyl)-benzo-[b]-thien-3-yl] [4-[2-(1-piperidinyl)ethoxy]phenyl] methanone (6.37 g, 12.7 mmol) in 52 ml of 1,2-dichloroethane. The resulting solution is heated to 35° C. After about 16 hours the reaction is complete. Methanol (30 ml) is added to the reaction mixture over a 20 minute period, causing the methanol to reflux. The resulting slurry was stirred at 25° C. After 1 hour, the crystalline product is filtered, washed with cold methanol (8 ml), and dried at 40 ° C. in vacuo to give 5.14 g of the title compound. mp 225° C.
WORKUP
后处理
- customcondensed into a cold graduated cylinder (2.8 ml)
- temperatureto reflux
- waitAfter 1 hour
- filtrationthe crystalline product is filtered
- washwashed with cold methanol (8 ml)
- customdried at 40 ° C. in vacuo