反应详情

A mixture of 18.6 g (93.5 mmol) 4-bromomethyl-1,2-dimethyl-benzene, 25.0 g (93.5 mmol) ethyl(diphenylmethylidene-amino)-acetate, 3.29 g (10.0 mmol) tetrabutylammonium bromide, 41.3 g (250 mmol) K2CO3×1.5H2O and 600 mL acetonitrile was refluxed overnight. The reaction mixture was filtered, the filtrate was evaporated down under reduced pressure, the residue was taken up in 500 mL diethyl ether and combined with 250 mL semiconc. HCl with vigorous stirring. Then the organic phase was separated off, the aqueous phase was extracted twice with diethyl ether and neutralised by the addition of solid NaHCO3. The aqueous phase was extracted by shaking three times with 200 mL EtOAc, the combined organic phases were washed once with water, dried over Na2SO4, filtered and evaporated down under reduced pressure.

1. temperaturewas refluxed overnight
2. filtrationThe reaction mixture was filtered
3. customthe filtrate was evaporated down under reduced pressure
4. customThen the organic phase was separated off
5. extractionthe aqueous phase was extracted twice with diethyl ether
6. additionneutralised by the addition of solid NaHCO3
7. extractionThe aqueous phase was extracted
8. washthe combined organic phases were washed once with water
9. dry with materialdried over Na2SO4
10. filtrationfiltered
11. customevaporated down under reduced pressure