HRID1501120
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To a solution of 1,1,1-trifluoropentane-2,4-dione (5.8 g, 37.7 mmol) in methanol (20 mL) was added malononitrile (5 g, 75 mmol) and then the mixture was heated to reflux. The mixture was maintained at the same temperature for 12 hours. The resultant mixture was cooled to room temperature, and then filtered. The solid was washed with methanol to give pure 2-hydroxy-6-methyl-4-(trifluoromethyl)nicotinonitrile (3 g, 40%). 1H NMR (300 MHz, d6-DMSO): δ 13.36 (s, 1H), 6.65 (s, 1H), 2.38 (s, 3H).
WORKUP
后处理
- temperaturethe mixture was heated to reflux
- temperatureThe mixture was maintained at the same temperature for 12 hours
- filtrationfiltered
- washThe solid was washed with methanol