HRID2303375

反应详情

EQUATION

反应方程式

HRID 2303375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1280 mg (2.2 mmol) of [2-(4-Methoxyphenyl)-6-methoxybenzo[b]thien-3-yl][4-(8-bromo-octyloxy)phenyl]methanone and 470 mg (6.6 mmol) of pyrrolidine were dissolve in 20 mL of dimethylformamide (DMF). The reaction mixture was heated to 100° C. and stirred under a nitrogen atmosphere. After 30 minutes, the reaction was allowed to cool and evaporated to dryness in vacuo. The crude product was chromatographed on a silica gel column eluted with a linear gradient begining with CHCl3 and ending with CHCl3—MeOH (19:1) (v/v). The desired fractions were determined by tlc, combined, and evaporated to dryness. This yielded 890 mg (72%) of the title compound as a tan, amorphous powder.

WORKUP

后处理

  1. temperatureto cool
  2. customevaporated to dryness in vacuo
  3. customThe crude product was chromatographed on a silica gel column
  4. washeluted with a linear gradient
  5. customevaporated to dryness