反应详情

温度

50 °C

1H-NMR (CDCl3): δ=2.35 (s, 3H); 2.65 (s, 3H); 6.79-7.84 (m, 8H) ppm. b) 38.7 g (0.43 mol) of dimethyl carbonate are added to a suspension of 10.3 g (0.43 mol) of sodium hydride in 230 ml of THF and then, at 50° C., a solution of 67.2 g (0.30 mol) of 2-(3-methylphenoxy)acetophenone is added dropwise. The mixture is stirred at 50° C. for 3 hours, left to cool, 60 ml of methanol are added, and the mixture is stirred at room temperature overnight. It is acidified (pH 2) with 10 percent hydrochloric acid and extracted with MTB ether. The organic phase is washed with water, dried and concentrated. 79.5 g (93% yield) of methyl 2-(3-methylphenoxy)benzoylacetate remain as dark oil.

1. waitleft
2. temperatureto cool
3. stirringthe mixture is stirred at room temperature overnight
4. extractionextracted with MTB ether
5. washThe organic phase is washed with water
6. customdried
7. concentrationconcentrated