反应详情

A solution of 200 mg (0.65 mmol) (S)-7-amino-5-(2,2,2-trifluoro-ethyl)-5H,7H-dibenzo[b,d]azepin-6-one and 150 mg (0.65 mmol) (RS)-2-hydroxy-2-methyl-N-(3,3,3-trifluoro-propyl)-malonamic acid in 7 ml tetrahydrofuran were cooled to 0° C. and 102 mg (0.65 mmol) 1-hydroxy-benzotriazole hydrate, 228 μl (1.31 mmol) diisopropylethylamine and 128 mg (0.65 mmol) N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimide hydrochloride were added. Stirring was continued overnight at room temperature. Removal of the solvent by distillation and chromatography on silicagel with ethylacetate/heptane (gradient 1/4 to 4/1) yielded 220 mg (65%) (R/S)-2-hydroxy-2-methyl-N-[(S)-6-oxo-5-(2,2,2-trifluoro-ethyl)-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl]-N′-(3,3,3-trifluoro-propyl)-malonamide as a white solid, MS (m/e): 518.2 (M+H)+.

1. customRemoval of the solvent
2. distillationby distillation and chromatography on silicagel with ethylacetate/heptane (gradient 1/4 to 4/1)