反应详情

温度

4 °C

A solution of 4.05 kg of (E)-2(R)-[1(S)-(tert-butoxycarbonyl)-4-phenyl-3-butenyl]-4-methylvaleric acid in 12 l of dimethylformanide was cooled to 4° C., treated with 1.97 kg of hydroxybenzotriazole hydrate and 2.466 kg of 1-ethyl-3-(3-dimethylaminopropyl)carbodimide hydrochloride and stirred for 2 hours at 4° C. 3.895 kg of isobutylhydrazine ditosylate salt were added followed by 2.36 l of N-methyl-morpholine. The mixture was stirred for 2 hours at 4° C. and for 50 hours at room temperature, diluted with 12 l of 2M hydrochloric acid and 12 l of methyl tert.butyl ether and the organic layer was separated. The organic phase was washed with water, saturated sodium hydrogen carbonate solution and water and then evaporated to give a dark cream colored solid. Recrystallization from hexane gave 2.47 kg of (E)-2(R)-[1(S)-(tert-butoxycarbonyl)-4-phenyl-3-butenyl]-2′-isobutyl-4-methylvalerohydrazide in the form of a cream colored solid.

1. stirringThe mixture was stirred for 2 hours at 4° C. and for 50 hours at room temperature
2. customthe organic layer was separated
3. washThe organic phase was washed with water, saturated sodium hydrogen carbonate solution and water
4. customevaporated
5. customto give a dark cream
6. customRecrystallization from hexane