反応 #336840

反応方程式

5,6-dichloro-2-cyclopropyl-4-pyrimidinecarboxylic acid

product

5,6-dichloro-2-cyclopropyl-4-pyrimidinecarboxylic acid

ammonia

→

title product

6-amino-5-chloro-2-cyclopropyl-4-pyrimidinecarboxylic acid

溶媒

water

反応条件

後処理

1. 1
   濃縮The solution was concentrated at 50° C.
2. 2
   その他70 torr (9.3 kPa) pressure to about half volume to remove most of the excess ammonia
3. 3
   温度cooled to 5° C.
4. 4
   ろ過filtered
5. 5
   その他The isolated solid was dried in a vacuum oven

実験手順

A mixture of 5,6-dichloro-2-cyclopropyl-4-pyrimidinecarboxylic acid (i.e. the product of Step C1 or C2) (280 g, 1.2 mol), water (1.26 L) and aqueous ammonia (28%, 350 g, 5.76 mol) was heated at 80° C. for 5 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 1-2 with aqueous hydrochloric acid, cooled to 5° C. and filtered. The isolated solid was dried in a vacuum oven to afford the title product (270 g), a compound of the present invention.

出典