反应详情

To a mixture of 3-benzyloxy-4-bromo-phenylamine (55.7 g, 0.168 mol) and ethyl acetoacetate (23.4 mL, 0.185 mol) in cyclohexane was added toluene-4-sulfonic acid monohydrate (0.320 g, 1.68 mmol) The reaction mixture was refluxed during 6 h and the water was azeotropically removed. The reaction mixture was then partitioned between ethyl acetate and an aqueous solution of sodium hydrogenocarbonate. The organic layer was washed with brine, dried over sodium sulfate, filtered and the solvents were evaporated under vacuum. 69.6 g of the title compound were obtained. Black oil, ISP-MS: m/e=392.2 ([M+H]+).

1. temperaturewas refluxed during 6 h
2. customthe water was azeotropically removed
3. customThe reaction mixture was then partitioned between ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customthe solvents were evaporated under vacuum