反应详情

温度

0 °C

To a mixture of D,L-serine, methyl ester (5.0 g, 32.14 mmol) and triethylamine (15.7 ml, 0.012 mmol) in methylene chloride (100 ml), cooled to 0° C., was added, in portions, 4-methoxybenzenesulfonyl chloride (6.64 g, 32.14 mmol). The mixture was then stirred under argon at room temperature for 48 hours. The reaction was diluted with methylene chloride (100 ml), washed with water (60 ml), 2N citric acid (60 ml), saturated sodium chloride (60 ml), and dried over anhydrous sodium sulfate. The solvent was removed in vacuo to give a solid. Crystallization from ethyl acetate gave 5.0 g (54%) of the product as white crystals, mp 92-94° C.

1. washwashed with water (60 ml), 2N citric acid (60 ml), saturated sodium chloride (60 ml)
2. dry with materialdried over anhydrous sodium sulfate
3. customThe solvent was removed in vacuo
4. customto give a solid
5. customCrystallization from ethyl acetate