反应详情

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

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