反应详情

To 10.8 g (0.10 mole) methoxybenzene and 13.9 g. (0.09 mole) phenylacetyl chloride in 1.0 1. methylene chloride there are added, by small amounts, 13.3 g. (0.10 mole) aluminium chloride at room temperature and with strong agitation. The reaction mixture is agitated for a further 2 hours and then is poured onto ice and 50 ml. hydrochloric acid are added. After separation of the organic phase, the aqueous solution is shaken out twice with 500 ml. methylene chloride each time, the combined organic phases are washed with water and the solvent is removed in vacuo. The smeary residue is freed of the volatile components by steam distillation and the remaining solid is crystallized from ethanol after filtration and washing with water. Obtained are colorless crystals having a melting point of 75° C.; Rf 0.7 [CHCl3 /CH3OH (9/1)]; yield: 18.3 g. (90%).

1. customat room temperature
2. additionis poured onto ice and 50 ml
3. customAfter separation of the organic phase
4. stirringthe aqueous solution is shaken out twice with 500 ml
5. washmethylene chloride each time, the combined organic phases are washed with water
6. customthe solvent is removed in vacuo
7. distillationThe smeary residue is freed of the volatile components by steam distillation
8. customthe remaining solid is crystallized from ethanol
9. filtrationafter filtration
10. washwashing with water
11. customObtained