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 dimethylformamide was cooled to 4° C. and treated with 1.97 kg of hydroxybenzotriazole hydrate and 2.466 kg of 1-ethyl-3-(3-dimethylaminopropyl)carbodimide hydrochloride and the solution was stirred for 2 hours at 4° C. 3.895 kg of isobutylhydrazine di-tosylate salt were added followed by 2.36 1 of N-methylmorpholine 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 phase was separated. The organic phase was washed with water, saturated sodium hydrogen carbonate solution and water and then evaporated to give a dark cream solid. Recrystallization from hexane gave 2.47 kg of (E)-2(R)-[1 (S)-(tert-butoxycarbonyl)-4-phenyl-3-butenyl]-2′-isobutyl-4-methyl-valerohydrazide in the form of a cream solid.

1. stirringwas stirred for 2 hours at 4° C. and for 50 hours at room temperature
2. customthe organic phase 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 solid
6. customRecrystallization from hexane