HRID3910

反应详情

EQUATION

反应方程式

HRID 3910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.1 Parts of dimethylamine hydrochloride was added to a solution of 2.3 parts of sodium in 20 parts of methanol. The resulting mixture was added dropwise with stirring over about 10 minutes to a solution of 9.9 parts of 2-amino-4-chloro-6-chloromethylpyrimidine in 50 parts of methanol. The reaction was monitored by TLC and when reaction was complete the solvent was evaporated and the residue stirred with about 20 parts of water. The solid obtained was filtered and dried. The product was purified by chromatography on silica, eluted with ethyl acetate, followed by sublimation at 110° C./0.04 mb to give 2-amino-4-chloromethyl-6-dimethylaminopyrimidine m.p. 127°-129° C.

WORKUP

后处理

  1. additionThe resulting mixture was added dropwise
  2. customThe reaction was monitored by TLC and when reaction
  3. customwas evaporated
  4. customThe solid obtained
  5. filtrationwas filtered
  6. customdried
  7. customThe product was purified by chromatography on silica
  8. washeluted with ethyl acetate
  9. customfollowed by sublimation at 110° C.