反应详情

温度

-10 °C

To a suspension of 3-hydroxy-7beta-phenylacetylaminocepham-4-carboxylic acid diphenylmethyl ester (2) in dichloromethane (13 parts) cooling at -10° C. under nitrogen are added triethylamine (4 equivalents) and then methanesulfonyl chloride (2.0 equivalents) at -10° C. over 7 minutes. The produced methanesulfonate ester (3) solution is let react at -10° C. for 30 minutes, and diluted with dichloromethane, washed with water, 5% sulfuric acid, and water, dried over sodium sulfate, and concentrated. The residue is crystallized from methanol (4 parts) to give 7beta-phenylacetylamino-3-cephem-4-carboxylic acid diphenylmethyl ester (6). (Yield: 75.4%).

1. washwashed with water, 5% sulfuric acid, and water
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated
4. customThe residue is crystallized from methanol (4 parts)