HRID51499

反应详情

EQUATION

反应方程式

HRID 51499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidine (906 mg), sodium hydride (120 mg, of a 60% dispersion in mineral oil) and dry dimethylformamide (30 ml) was stirred at ambient temperature under nitrogen for 30 minutes. Ethyl bromoacetate (0.5 g) in dimethylformamide (10 ml) was added over 5 minutes at 0-5° C. with stirring. The mixture was stirred for 30 minutes at ambient temperature and then allowed to stand for 18 hours. The mixture was evaporated under vacuum and the residue was triturated with water and ether. The solid obtained was collected by filtration, washed with water and then with ether to give ethyl 2-[4-amino-5-(4-phenoxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-7-yl]acetate, m.p. 161-161.3° C.

WORKUP

后处理

  1. stirringThe mixture was stirred for 30 minutes at ambient temperature
  2. customThe mixture was evaporated under vacuum
  3. customthe residue was triturated with water and ether
  4. customThe solid obtained
  5. filtrationwas collected by filtration
  6. washwashed with water