반응 #2487452

반응 방정식

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

용매

ethyl acetate

반응 조건

후처리

1. 1
   세척washed with hydrochloric acid (1 M, 25 mL) and water (25 mL)
2. 2
   건조The organic phase was dried over MgSO4
3. 3
   여과filtered
4. 4
   농축concentrated under reduced pressure (0.98 g)

실험 절차

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+).

출처