反应详情

A mixture of 3-hydroxybenzamide (0.5 g, 3.65 mmol), 1,5-dibromopentane (1.82 g, 1.1 ml, 7.3 mmol) and potassium carbonate (500 mg, 3.65 mmol) was refluxed (2 h) in acetonitrile (18 ml) until the reaction was complete by TLC. The solvent was then removed by rotary evaporation to leave a white sticky solid which was chromatographed (10% methanol in dichloromethane on silica) to give a white solid. This was recrystallised from a mixture of petrol and ethyl acetate to give white flaky crystals (0.744 g, 2.6 mmol, 70% yield). mp 98-99° C.

1. customThe solvent was then removed by rotary evaporation
2. customto leave a white sticky solid which
3. customwas chromatographed (10% methanol in dichloromethane on silica)
4. customto give a white solid
5. customThis was recrystallised from a mixture of petrol and ethyl acetate