HRID237384

反应详情

EQUATION

反应方程式

HRID 237384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Hydrochloric acid was added to a solution of 2-Amino-4-(2,4-dichloro-5-(2,2-diethoxyethoxy)-phenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in THF and the solution stirred for ˜18 hrs. Morpholine was added and the solution stirred, sodium triacetoxyborohydride was added and the resulting suspension stirred for ˜18 hrs. Dichloromethane was added and the mixture washed with aqueous ammonia (0.880), water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a pale yellow solid. The crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane.

WORKUP

后处理

  1. stirringthe solution stirred
  2. stirringthe resulting suspension stirred for ˜18 hrs
  3. washthe mixture washed with aqueous ammonia (0.880), water and saturated aqueous sodium chloride solution
  4. dry with materialThe solution was dried over anhydrous sodium sulphate
  5. concentrationconcentrated to a pale yellow solid
  6. customThe crude product was purified by chromatography on silica eluting with mixtures of ethyl acetate and hexane