反应详情

p-Chlorobenzoyl chloride (0.91 g) and triethylamine (0.91 ml) were added at 5° C. to a solution of 0.85 g of isomer (i) of the 2-(2-cyanoethyl)alanine methyl ester in dichloromethane (20 ml), and the resulting mixture was stirred at 0°-5° C. for 2 hours. The reaction mixture was then washed with water (20 ml) and the organic layer was dried over magnesium sulphate. The solvent was distilled off and the residue was purified by silica gel Lobar column chromatography (eluent: 1/1 cyclohexane/ethyl acetate; flow rate: 12 ml/minute), giving 1.13 g of isomer (i) of the desired product as a colourless powder.

1. washThe reaction mixture was then washed with water (20 ml)
2. dry with materialthe organic layer was dried over magnesium sulphate
3. distillationThe solvent was distilled off
4. customthe residue was purified by silica gel Lobar column chromatography (eluent: 1/1 cyclohexane/ethyl acetate; flow rate: 12 ml/minute)