反应详情

To a solution of 10-[(2-methyl-2′-trifluoromethyl-[1,1′-biphenyl]-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxylic acid of Example 1, Step F (1.2 g, 2.44 mmol) and 3-methylamino-1,2-propanediol (0.32 g, 3.04 mmol) in N,N-dimethyl formamide (10 mL) was added 1-hydroxybenzotriazole (0.36 g, 2.66 mmol) and 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.52 g, 2.71 mmol) followed by N,N-diisopropylethyl amine (0.64 mL, 3.67 mmol). The reaction mixture was stirred overnight, diluted with ethyl acetate and washed with water and saturated aqueous sodium bicarbonate. The organic phase was then dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give a brown foam. Purification by flash chromatography using a solvent system of 5% methanol in chloroform gave a white foam, which was crystallized from ethyl acetate to provide 1.15 g of title product as a white solid, m.p. 169-172° C.

1. washwashed with water and saturated aqueous sodium bicarbonate
2. dry with materialThe organic phase was then dried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto give a brown foam
6. customPurification by flash chromatography
7. customgave a white foam, which
8. customwas crystallized from ethyl acetate