反应详情

温度

100 °C

1,2-Hydrazinedicarboxaldehyde (0.095 g, 1.1 mmol) and then, drop by drop, chlorotrimethylsilane (0.69 mL, 5.4 mmol) and triethylamine (0.35 mL, 2.5 mmol) were added to a suspension of 1-(6-amino-4-chloro-3′-fluoro-5-methylbiphenyl-2-yl)ethanone (0.10 g, 0.36 mmol) in pyridine (2 mL). The mixture was heated at 100° C. overnight. Evaporation at reduced pressure of the solvent yielded a solid that was treated with water and extracted with dichloromethane. The extracts were dried over sodium sulfate and concentrated. The reside was purified on silica gel, eluting with 0 to 50% ethyl acetate in hexane, then 0 to 10% methanol in dichloromethane, to give the desired product (44 mg, 37%). LCMS calculated for C17H14ClFN3O (M+H)+: m/z=330.1. found: 330.0.

1. customEvaporation at reduced pressure of the solvent
2. customyielded a solid
3. extractionextracted with dichloromethane
4. dry with materialThe extracts were dried over sodium sulfate
5. concentrationconcentrated
6. customThe reside was purified on silica gel
7. washeluting with 0 to 50% ethyl acetate in hexane