HRID249657

反应详情

EQUATION

反应方程式

HRID 249657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 5,6-dichloro-2-cyclopropyl-4-pyrimidinecarboxylic acid (i.e. the product of Step C1 or C2) (5.1 g, 22 mmol), water (30 mL) and aqueous ammonia (28%, 8 g, 130 mmol) was heated at 80° C. for 3 h. The solution was concentrated at 50° C. and 70 torr (9.3 kPa) pressure to about half volume to remove most of the excess ammonia. The resulting slurry was stirred at 20° C., acidified to pH 2 with aqueous hydrochloric acid, cooled to 5° C. and filtered. The isolated solid was dried in a vacuum oven to afford the title product (4.2 g), a compound of the present invention.

WORKUP

后处理

  1. concentrationThe solution was concentrated at 50° C.
  2. custom70 torr (9.3 kPa) pressure to about half volume to remove most of the excess ammonia
  3. temperaturecooled to 5° C.
  4. filtrationfiltered
  5. customThe isolated solid was dried in a vacuum oven