HRID904562

反应详情

EQUATION

反应方程式

HRID 904562 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 10-oxo-10H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxylic acid (6.0 g., 0.024 mol) and 1,1'-carbonyldiimidazole (4.0 g., 0.024 mol) in dimethylformamide (120 ml) is heated at 110° C. for 2.5 hours under nitrogen. The solution is cooled in an ice bath and anhydrous ammonia is bubbled through for 15 minutes. The mixture is stirred at ice bath temperature for 2 hours and at room temperature for one hour. The precipitate is filtered off, washed with tetrahydrofuran and dried to give the product (5.2 g.), mp 340° C. (dec).

WORKUP

后处理

  1. temperatureThe solution is cooled in an ice bath
  2. customanhydrous ammonia is bubbled through for 15 minutes
  3. waitat room temperature for one hour
  4. filtrationThe precipitate is filtered off
  5. washwashed with tetrahydrofuran
  6. customdried
  7. customto give the product (5.2 g.), mp 340° C. (dec)