反应详情

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.80 g) was added to a solution of 4-dimethylaminopyridine (0.04g) and Intermediate 10 (0.54 g) in dichloromethane (30 ml) and the solution was stirred for 30 min, then a solution of Intermediate 14 (0.50 g) in dichloromethane (5 ml) was added and the mixture was stirred overnight. The solvent was removed in vacuo and the resulting slurry dissolved in ethyl acetate (100 ml), washed with water (10 ml), aqueous sodium bicarbonate (10 ml) and brine (10 ml), dried over magnesium sulphate (1 g) and the solvent removed in vacuo. The resulting oil was purified by flash chromatography (silica, eluent 30% ethyl acetate/hexane) to yield the title compound as a yellow solid (0.26 g).

1. stirringthe mixture was stirred overnight
2. customThe solvent was removed in vacuo
3. dissolutionthe resulting slurry dissolved in ethyl acetate (100 ml)
4. washwashed with water (10 ml), aqueous sodium bicarbonate (10 ml) and brine (10 ml)
5. dry with materialdried over magnesium sulphate (1 g)
6. customthe solvent removed in vacuo
7. customThe resulting oil was purified by flash chromatography (silica, eluent 30% ethyl acetate/hexane)