HRID3909

反应详情

EQUATION

反应方程式

HRID 3909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22.0 Parts of 2-amino-4-chloro-6-(2,2-dichlorovinyl)pyrimidine was dissolved in 500 parts of dry methanol and stirred whilst a solution of sodium methoxide, prepared by dissolving 4.6 parts of sodium in 200 parts of dry methanol, was added dropwise, over 30 minutes at ambient temperature. The resulting solution was stirred for 4 hours by which time all the starting material had been consumed. The product was precipitated by the addition of water, filtered and dried. The solid obtained was purified by chromatography on silica using diethyl ether as eluent. Final purification was effected by recrystallisation from carbon tetrachloride to give 2-amino-4-(2,2-dichlorovinyl)-6-methoxypyrimidine m.p. 90°-91° C.

WORKUP

后处理

  1. customprepared
  2. additionwas added dropwise, over 30 minutes at ambient temperature
  3. customhad been consumed
  4. customThe product was precipitated by the addition of water
  5. filtrationfiltered
  6. customdried
  7. customThe solid obtained
  8. customwas purified by chromatography on silica
  9. customFinal purification
  10. customwas effected by recrystallisation from carbon tetrachloride