反应详情

温度

85 °C

A mixture of 2,2,2-trichloro-1-{10-[(2,2′-dimethyl-1,1′-biphenyl-4-yl)carbonyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone of Example 9 (0.26 mmol), dimethylsulfoxide (100 uL) and [5-(4-methoxyphenyl)-1,2,4-oxadiazol-3-yl]methylamine of Step A (0.546 mmol) in acetonitrile (2.5 mL) was heated to 85° C. for 16 hours. After cooling the solvent was evaporated and the residue was taken up in dichloromethane (10 mL). This was washed with water (2×), dried over anhydrous sodium sulfate, and evaporated. The residue was purified by HPLC (Normal phase, Luna CN bonded packing) and crystallized from ethyl acetate/hexane, m.p. 133-135° C.

1. temperatureAfter cooling the solvent
2. customwas evaporated
3. washThis was washed with water (2×)
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated
6. customThe residue was purified by HPLC (Normal phase, Luna CN bonded packing)
7. customcrystallized from ethyl acetate/hexane, m.p. 133-135° C.