反应详情

In 100 ml of water was suspended 10 g of 7-aminocephalosporanic acid (hereinafter abbreviated as "7-ACA"). The pH of the suspension was maintained at 12.5 to 13.4 by gradual addition of 2N-sodium hydroxide solution under ice-cooling and stirring. The mixture was further stirred for 2 hours, and adjusted to pH 3.4 with 4N-hydrochloric acid after confirming the disappearance of the starting material (7-ACA) by TLC. The precipitating crystals were collected by filtration, washed with water and acetone and dried over phosphorus pentoxide under reduced pressure to give 5.4 g of 7β-amino-3-hydroxymethyl -3-cephem-4-carboxylic acid as pale yellow crystals.

1. temperaturecooling
2. stirringThe mixture was further stirred for 2 hours
3. filtrationThe precipitating crystals were collected by filtration
4. washwashed with water and acetone
5. dry with materialdried over phosphorus pentoxide under reduced pressure