反应详情

温度

82.5 °C

A mixture of 2,2,2-trichloro-1-{10-[(2′-methoxy-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone of Example 1 (0.517 g, 0.985 mmole) and (R)-(−)-2-amino-2-phenylethanol (0.276 g, 20 mmole), dimethylsulfoxide (2.8 mmole) and triethylamine (0.213 g, 2.1 mmole) in acetonitrile (10 mL) was heated at 80-85° C. for 22 hours. The residue left upon removal of the solvent was taken up in 15 mL of dichloromethane, washed with brine, dried over anhydrous magnesium sulfate and concentrated to give a tan solid. Purification by flash chromatography on silica gel Merck-60 using a gradient of 0 to 25% ethyl acetate in dichloromethane provided a light yellow solid (0.283 g). Recrystallization from ethyl acetate/hexane gave the title compound as off-white needles, m.p. 195-196° C. MS [(+)ESI, m/z]: 558.14 [M+H]+

1. waitThe residue left upon removal of the solvent
2. washwashed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customto give a tan solid
6. customPurification by flash chromatography on silica gel Merck-60