反应详情

温度

-30 °C

To a suspension of 7-benzoylamino-3-(1-methyl-1-pyrrolidinio)methyl-3-cephem-4-carboxylate (15 g) in a mixture of dichloromethane (300 ml) and N,N-dimethylaniline (41.7 g) was added dropwise trimethylsilyl chloride (31.2 g) at 5° C. After being stirred for 1 hour at 5°-10° C., the mixture was cooled up to -30° C. and then phosphorus pentachloride (11.9 g), was added thereto. After the mixture was stirred for 1 hour at -20°~-30° C., a mixture of isobutyl alcohol (21.2 g) and 1,3-propanediol (21.8 g) is dichloromethane (150 ml) cooled at -30° C. was added to the reaction mixture. The mixture was stirred for 1 day at room temperature to give a residue, which was collected by filtration, washed with dichloromethane, acetone and diisopropyl ether successively and dried over phosphorus pentoxide to give 7-amino-3-(1-methyl-1-pyrrolidinio)methyl-3-cephem-4-carboxylate dihydrochloride.

1. stirringAfter the mixture was stirred for 1 hour at -20°~-30° C.
2. temperaturecooled at -30° C.
3. additionwas added to the reaction mixture
4. stirringThe mixture was stirred for 1 day at room temperature
5. customto give a residue, which
6. filtrationwas collected by filtration
7. washwashed with dichloromethane, acetone and diisopropyl ether successively
8. dry with materialdried over phosphorus pentoxide