反应详情

396 mg (1.1 mmol) N-[(9H-fluoren-9-ylmethoxy)carbonyl]-N-methyl-L-valine were dissolved in 20 ml DMF and 365 mg (1 mmol) tert.-butyl-(3R,4S,5S)-3-methoxy-5-methyl-4-[methyl(L-valyl)amino]heptanoate (intermediate 2), 234 mg (1.2 mmol) 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 187 mg (1.2 mmol) 1-hydroxy-1H-benzotriazol hydrate were added in succession. The mixture was stirred overnight at RT. The mixture was then poured into a solution of semi-saturated aqueous ammonium chloride and ethyl acetate. The organic phase was separated off, washed successively with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution, then dried over magnesium sulphate, filtered and evaporated. The residue was used directly in the next step, without purification.

1. customThe organic phase was separated off
2. washwashed successively with saturated sodium hydrogen carbonate solution and saturated sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. customevaporated
6. customThe residue was used directly in the next step, without purification