反应详情

To oxalyl chloride (1.01 g) in dichloromethane (10 ml) at -70° C. was added dimethylsulphoxide (1.23 g) in dichloromethane (6 ml). To the resulting mixture was dropwise added a solution of α-(1-phenylethenyl)-2,4-dichlorobenzenemethanol (2.07 g) in dichloromethane (6 ml). Triethylamine (2.17 g) was added to the reaction mixture and the resulting mixture was stirred for an additional 20 minutes and then allowed to warm to room temperature. The reaction mixture was washed with water and the organic phase separated and concentrated under reduced pressure. The resulting residue was redissolved in ethyl acetate, washed with water, dried over anhydrous magnesium sulphate. The solvent removed under reduced pressure to yield 1-(2,4-dichlorophenyl)-2-(4-methylphenyl)propen-1-one (δ (CDCl3), 5.92 (1H,s) 6.16 (1H,s) and 7.1-7.3 (10H,m) p.p.m.) as an oil having the formula: ##STR19##

1. washThe reaction mixture was washed with water
2. customthe organic phase separated
3. concentrationconcentrated under reduced pressure
4. dissolutionThe resulting residue was redissolved in ethyl acetate
5. washwashed with water
6. dry with materialdried over anhydrous magnesium sulphate
7. customThe solvent removed under reduced pressure