HRID357500

反应详情

EQUATION

反应方程式

HRID 357500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound No. 46. A suspension of 4-phenylamino-2-amino-6-methylpyrimidine, Compound No. 45, (0.25 g) in ethanol (4 mL) was treated with methyl methanesulfonate (0.090 g) and heated at reflux for 5 days. Additional methyl methanesulfonate (0.090 g) was added and the mixture refluxed another 2 days. Concentration and recrystallization from a mixture of methanol, ethyl acetate, and tert-butyl ethyl ether gave 0.10 g of 4-phenylamino-2-amino-1,6-dimethylpyrimidinium methanesulfonate.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 5 days
  3. temperaturethe mixture refluxed another 2 days
  4. concentrationConcentration and recrystallization
  5. additionfrom a mixture of methanol, ethyl acetate, and tert-butyl ethyl ether