HRID1808349

反应详情

EQUATION

反应方程式

HRID 1808349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

TEA (28.66 mmol, 4 equiv.) was added at 0° C. to a solution of methyl 4-((benzyl(2-chloroethyl)amino)methyl)-1H-imidazole-5-carboxylate (7.16 mmol, 1 equiv.) in acetonitrile (50 ml). The resulting mixture was heated for 16 h at 80° C. It was then cooled and filtered, and the filtrate was concentrated in vacuo. The crude product was taken up in DCM and sat. sodium hydrogen carbonate solution, and the organic phase was dried and concentrated in vacuo. The resulting crude product was purified by column chromatography (silica gel, 5% MeOH in DCM), and the desired product was thus obtained in the form of a brown solid. Yield: 64%

WORKUP

后处理

  1. temperatureIt was then cooled
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated in vacuo
  4. dry with materialsat. sodium hydrogen carbonate solution, and the organic phase was dried
  5. concentrationconcentrated in vacuo
  6. customThe resulting crude product was purified by column chromatography (silica gel, 5% MeOH in DCM)