반응 #336841

반응 방정식

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

D2

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

thionyl chloride

methanol

ammonia

water

→

title product

methyl 6-amino-5-chloro-2-cyclopropyl-4-pyrimidinecarboxylate

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도at reflux for 24 h
3. 3
   온도the reaction mixture was heated
4. 4
   온도at reflux for 16 h
5. 5
   온도After the mixture was cooled
6. 6
   기타the solid was isolated by filtration
7. 7
   세척washed with water
8. 8
   기타dried in a vacuum oven at 40° C.

실험 절차

To a solution of 6-amino-5-chloro-2-cyclopropyl-4-pyrimidinecarboxylic acid (i.e. the product of Step D1 or D2 of Example 2) (2.0 g, 8.5 mmol) in methanol (20 mL) was added dropwise thionyl chloride (4 mL, 70 mmol). The mixture was heated at reflux for 24 h. Concentrated sulfuric acid (5 drops) was added, and the reaction mixture was heated at reflux for 16 h. After the mixture was cooled, water (30 mL) was added, and aqueous ammonia (28%, 10 mL) was added dropwise. The mixture was cooled to 5° C., and the solid was isolated by filtration, washed with water and dried in a vacuum oven at 40° C. to afford the title product (2.3 g), a compound of the present invention.

출처