반응 #336840

반응 방정식

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

용매

water

반응 조건

후처리

1. 1
   농축The solution was concentrated at 50° C.
2. 2
   기타70 torr (9.3 kPa) pressure to about half volume to remove most of the excess ammonia
3. 3
   온도cooled to 5° C.
4. 4
   여과filtered
5. 5
   기타The isolated solid was dried in a vacuum oven

실험 절차

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.

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