HRID1638560

反应详情

EQUATION

反应方程式

HRID 1638560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The sodium salt of diethylmalonate was generated from 0.35 g of NaH (50% oil dispersion) and 1.1 mL of diethyl malonate in 15 mL of dried DMF with ice cooling. To the above mixture was added 2 g of 1-(4-nitrobenzyl)-2-chloromethylbenzimidazole and the mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate, washed with water, dried and concentrated in vacuo. The crude produce was purified by flash column chromatography (hexane/ethyl acetate, 1:1) to give a yellowish thick oil which was crystallized from absolute ethanol to give a white solid; m.p. 135°.

WORKUP

后处理

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated in vacuo
  4. customThe crude produce
  5. customwas purified by flash column chromatography (hexane/ethyl acetate, 1:1)
  6. customto give a yellowish thick oil which
  7. customwas crystallized from absolute ethanol
  8. customto give a white solid