HRID2407697

反应详情

EQUATION

反应方程式

HRID 2407697 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-(methylthio)-4-(phenylamino)pyrimidine-5-carboxylate (4.0 g, prepared according to the reported preparation in Barvian, M.; et al. J. Med. Chem. 2000, 43, 4606) in ethanol (50 mL) was treated with 2 N lithium hydroxide (50 mL) at room temperature for 16 hours. The reaction mixture was washed with ether and then brought to pH 6 via the addition of 1 N hydrochloric acid. The resulting precipitate was collected by filtration, azeotroped with toluene and dried under vacuum to obtain the title compound (2.2 g) having the following physical data.

WORKUP

后处理

  1. customaccording to the reported preparation in Barvian, M
  2. washThe reaction mixture was washed with ether
  3. additionbrought to pH 6 via the addition of 1 N hydrochloric acid
  4. filtrationThe resulting precipitate was collected by filtration
  5. customazeotroped with toluene
  6. customdried under vacuum