反应详情

6.92 g (25 mmol) 4-chloro-3',4'-dimethoxybenzophenone, 12.9 g (100 mmol) N-acetylmorpholine and 11.2 g (170 mmol) powdered potassium hydroxide (85%) were mixed well and allowed to stand at room temperature for 30 minutes, with occasional stirring. The viscous mass so obtained was then added to a vigorously stirred mixture of 100 ml water and 50 ml toluene. The toluene phase was dried and separated over a column containing 50 g silica gel using 150 ml each of 95:5, 90:10 and 80:20 toluene-acetone mixture as eluant. The fractions with an Rf value of 0.37 (Toluene/Acetone 7:3) were evaporated in a rotary evaporator, after which 0.8 g of the title compound were obtained by trituration with a little diisopropyl ether.

1. customThe viscous mass so obtained
2. dry with materialThe toluene phase was dried
3. customseparated over a column
4. additioncontaining 50 g silica gel using 150 ml each of 95:5, 90:10 and 80:20 toluene-acetone mixture as eluant
5. customThe fractions with an Rf value of 0.37 (Toluene/Acetone 7:3) were evaporated in a rotary evaporator