HRID1278471

反应详情

EQUATION

反应方程式

HRID 1278471 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

As described in Example 1, 5.82 g. of 2-phenylpropanenitrile, 2.04 g. of 50% sodium hydride, and 3.06 g. of 4-chloromethylimidazole hydrochloride were reacted in 40 ml. of dimethylformamide. The mixture was stirred for 5 hours at 100° C., and for 16 hours at ambient temperature. The solvent was then evaporated away under vacuum, and the residue was worked up as described in Example 1 to obtain 0.4 g. of crude free base. The product was purified by preparative thin layer chromatography on silica gel with ethyl acetate as the eluant. The purified product was converted to 0.11 g. of the hydrochloride salt of the desired product, m.p. 187°-189° C.

WORKUP

后处理

  1. waitfor 16 hours at ambient temperature
  2. customThe solvent was then evaporated away under vacuum
  3. customto obtain 0.4 g
  4. customThe product was purified by preparative thin layer chromatography on silica gel with ethyl acetate as the eluant