反应详情

To a solution of the carboxylic acid of step 2 (10.2 g, 36.9 mmol), L-Leucineamide hydrochloride (6.18 g, 40.5 mmol), EDCI hydrochloride (5.48 g, 40.6 mmol), and HOBT (5.48 g, 40.6 mmol) in 100 mL of anhydrous DMF, was added N-methylmorpholine (12.0 mL, 109 mmol). The reaction mixture was stirred at ambient temperature for 24 h, then added 300 mL of water and 400 mL of ethyl acetate. The organic layer was separated and washed with two 300 mL portions of a 0.5 M HCl solution, 300 mL of water, then dried over sodium sulfate, filtered and recrystallized from ethyl acetate/hexanes to give 13.2 g of [2-(1-Carbamoyl-3-methyl-butylcarbamoyl)-cyclohexyl]-carbamic acid benzyl ester as a white solid. Yield: 92%, MS: 412 (M+Na+), mp=188.0-189.5° C.

1. customThe organic layer was separated
2. washwashed with two 300 mL portions of a 0.5 M HCl solution, 300 mL of water
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. customrecrystallized from ethyl acetate/hexanes