反应 #2487452

反应方程式

2,3-difluoro-6-iodo-4-trifluoromethylbenzoic acid

4-chlorobenzamide hydrochloride

caesium carbonate

dimethylformamide

→

quinazolin-4-one

2-(4-Chlorophenyl)-5,6-difluoro-7-trifluoromethyl-3H-quinazolin-4-one

溶剂

ethyl acetate

反应条件

后处理

1. 1
   洗涤washed with hydrochloric acid (1 M, 25 mL) and water (25 mL)
2. 2
   干燥The organic phase was dried over MgSO4
3. 3
   过滤filtered
4. 4
   浓缩concentrated under reduced pressure (0.98 g)

实验过程

A suspension of crude 2,3-difluoro-6-iodo-4-trifluoromethylbenzoic acid (1.00 g), 4-chlorobenzamide hydrochloride (0.814 g, 4.26 mmol), copper (I) iodide (0.108 g), caesium carbonate (1.85 g, 5.68 mmol) in dimethylformamide (8 mL) were stirred under nitrogen at room temperature for 1 week. The reaction mixture was then diluted with ethyl acetate (100 mL) and washed with hydrochloric acid (1 M, 25 mL) and water (25 mL). The organic phase was dried over MgSO4, filtered and concentrated under reduced pressure (0.98 g). The reaction was repeated with crude 2,3-difluoro-6-iodo-4-trifluoromethylbenzoic acid (0.50 g) to afford an additional portion (0.57 g) of the quinazolin-4-one. LC-MS: 3.6 min, 361 (M+).

来源