反应详情

To a solution of the crude 4-methyl-2-[(5-phenyl-4H-1,2,4-triazol-3-yl)sulfanyl]pentanoic acid in DMF (10 mL) was added aminoacetonitrile hydrochloride (427 mg, 4.62 mmoles) and HATU (1.76 g, 4.62 mmoles). After stirring for 30 seconds, triethylamine (1.3 mL, 9.24 mmoles) was added in one portion. The reaction was stirred overnight, diluted with ethyl acetate and water. The organic phase was separated and washed twice with 1.2 N hydrochloric acid, brine and dried over magnesium sulfate. After concentration under reduced pressure, N-(cyanomethyl)-4-methyl-2-[(5-phenyl-4H-1,2,4-triazol-3-yl)sulfanyl]pentanamide was obtained. MS (−APCI): 328.2 [M−1]−.

1. stirringThe reaction was stirred overnight
2. customThe organic phase was separated
3. washwashed twice with 1.2 N hydrochloric acid, brine
4. dry with materialdried over magnesium sulfate
5. concentrationAfter concentration under reduced pressure