HRID1773513

反应详情

EQUATION

反应方程式

HRID 1773513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Trichloroacetyl isocyanate (2.0 g) was added to a solution of methyl 3-amino-4-methylthiophene-2-carboxylate (1.3 g) in acetonitrile (10 mL) and the resulting mixture was stirred for 15 minutes. The solid, which crashed out, was collected by filtration and suspended in methanol (5 mL), a solution of ammonia in methanol (7 M, 5 mL) was then added and the resulting mixture was heated at 70° C. for 15 minutes. The reaction mixture was cooled, the solid formed was collected by filtration, dried under reduced pressure to give 0.8 g of 7-methyl-1H-thieno[3,2-d]pyrimidine-2,4-dione.

WORKUP

后处理

  1. filtrationwas collected by filtration
  2. additiona solution of ammonia in methanol (7 M, 5 mL) was then added
  3. temperatureThe reaction mixture was cooled
  4. customthe solid formed
  5. filtrationwas collected by filtration
  6. customdried under reduced pressure