反应详情

A suspension of 5,8-dihydro-2-(4-formyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid (273 g) and triethylamine (299 ml) in dried dichloromethane (3500 ml) was stirred well at room temperature for one hour. To the suspension, isopropyl chloroformate (221 g) was added dropwise with cooling at 0°-10° C. and the reaction mixture was stirred for 2 hours. A solution of N-hydroxysuccinimide (207 g) in dimethylformamide (350 ml) was added to the mixture and the resulting mixture was kept at 5°-10° C. for additional 2 hours. The crystalline product was collected by filtration and washed successively with water (2000 ml) and acetone (2000 ml) to give N-[5,8-dihydro-2-(4-formyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carbonyloxy] succinimide (326 g). m.p. above 300° C.

1. temperaturewith cooling at 0°-10° C.
2. stirringthe reaction mixture was stirred for 2 hours
3. waitthe resulting mixture was kept at 5°-10° C. for additional 2 hours
4. filtrationThe crystalline product was collected by filtration
5. washwashed successively with water (2000 ml) and acetone (2000 ml)