HRID1750315
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 5-phenylthieno[2,3-d]pyrimidin-4(3H)-one (20 g, 88 mmol), 1,1,1-trifluoro-2-iodoethane (36.8 g, 175 mmol) and potassium carbonate (26.6 g, 193 mmol) in DMF (100 ml) was heated at 70° C. for 0.5 h and at 100° C. for 2 h. A further portion of 1,1,1-trifluoro-2-iodoethane (36.8 g, 175 mmol) was added and the resulting mixture was heated at 100° C. for a further 16 h. The reaction mixture was cooled down and diluted with water (750 ml) and the precipitate was filtered to give the title compound as a light yellow solid (13 g, 48%). LCMS RT=1.30 min, M+H+=311.1.
WORKUP
后处理
- temperaturethe resulting mixture was heated at 100° C. for a further 16 h
- temperatureThe reaction mixture was cooled down
- filtrationthe precipitate was filtered