反应详情

4-Bromomethylbenzoic acid (4.1 mmol), HOBt (4.1 mmol) and WSCD.HCI (4.1 mmol) are dissolved in dimethylformamide (7 ml) and stirred for 10 min. 2-Amino-4-methyl-pentanoic acid (cyano-dimethyl-methyl)-amide (4.1 mmol) is added in DMF (3 ml) and the reaction mixture is stirred at RT overnight. After evaporation of the solvent, the residue is extracted with ethyl acetate. The extract is washed with water, 10% citric acid, brine, sodium bicarbonate, brine and dried over magnesium sulfate and evaporated. The crude product is suspended in diethylether and the solid filtered of and dried (vacuum). A white powder with mp. 185-187° C., Rf=0.43 (n-hexane:ethyl acetate=1:1) is obtained.

1. stirringthe reaction mixture is stirred at RT overnight
2. customAfter evaporation of the solvent
3. extractionthe residue is extracted with ethyl acetate
4. washThe extract is washed with water, 10% citric acid, brine, sodium bicarbonate, brine
5. dry with materialdried over magnesium sulfate
6. customevaporated
7. filtrationthe solid filtered of and
8. customdried (vacuum)
9. customA white powder with mp. 185-187° C., Rf=0.43 (n-hexane:ethyl acetate=1:1) is obtained