反应详情

2-Bromo-5-chlorophenol (8 g), 2-bromo-N,N-dimethylpropionamide (6.66 g) and anhydrous potassium carbonate (2.6 g) in methyl iso-butyl ketone (100 ml) were refluxed with stirring overnight. The mixture was cooled to 50° and washed with 5% sodium hydroxide (2×20 ml) and then water (2×50 ml). The organic solution was dried and evaporated under reduced pressure to yield a pale red oil, which solidified on cooling. Recrystallisation from 50% aqueous ethanol gave the title compound, m.p. 76°-77°. Compounds 2, 9, 10 to 13, 17 and 21 were made by a similar procedure.

1. temperatureThe mixture was cooled to 50°
2. washwashed with 5% sodium hydroxide (2×20 ml)
3. customThe organic solution was dried
4. customevaporated under reduced pressure
5. customto yield a pale red oil, which
6. temperatureon cooling
7. customRecrystallisation from 50% aqueous ethanol