反应详情

A solution of methyl 3-methoxy-4-(2-methylallyloxy)benzoate (130 g, 0.55 mol) in NMP (500 mL) was heated to reflux for 6 h. TLC (EtOAc/petroleum ether=1/5) showed the reaction was complete. The mixture was washed with 1 N aq. HCl and extracted with EtOAc (250 mL×3). The combined organic phases were washed with brine (400 mL), dried over Na2SO4 and concentrated to give the product (150 g, 100%) as a brown oil. The oil was used directly to the next step without further purification.

1. temperatureto reflux for 6 h
2. washThe mixture was washed with 1 N aq. HCl
3. extractionextracted with EtOAc (250 mL×3)
4. washThe combined organic phases were washed with brine (400 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated