反应 #336841

反应方程式

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

反应条件

后处理

1. 1
   温度The mixture was heated
2. 2
   温度at reflux for 24 h
3. 3
   温度the reaction mixture was heated
4. 4
   温度at reflux for 16 h
5. 5
   温度After the mixture was cooled
6. 6
   其他the solid was isolated by filtration
7. 7
   洗涤washed with water
8. 8
   其他dried in a vacuum oven at 40° C.

实验过程

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.

来源