反応 #336842

反応方程式

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

D2

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

thionyl chloride

methanol

→

title product

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

反応条件

後処理

1. 1
   濃縮The mixture was concentrated to 25% of the original volume
2. 2
   workup.ADDITIONdiluted with water (100 mL)
3. 3
   workup.ADDITIONPhenolphthalein pH indicator was added
4. 4
   workup.ADDITION10% aqueous sodium hydroxide was added dropwise
5. 5
   温度with cooling at 10-20° C.
6. 6
   その他The solid was isolated by filtration
7. 7
   洗浄washed with water
8. 8
   その他dried in a vacuum oven at 50-60° C.

実験手順

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) (8.5 g, 40 mmol) in methanol (120 mL) was added dropwise with cooling thionyl chloride (15 mL, 200 mmol). The mixture was heated at 60° C. for 24 h. The mixture was concentrated to 25% of the original volume and diluted with water (100 mL). Phenolphthalein pH indicator was added, and 10% aqueous sodium hydroxide was added dropwise with cooling at 10-20° C. to bring the pH to 8-10. The solid was isolated by filtration, washed with water and dried in a vacuum oven at 50-60° C. to afford the title product (7.3 g), a compound of the present invention.

出典