反应详情

A mixture of 4-hydroxy-3-nitrophenyl benzoate (48.8 g, 0.19 mol), methyl bromoacetate (28.8 g, 0.19 mol), anhydrous potassium carbonate (33.8 g, 0.24 mol) and acetone (700 mL) was heated at reflux for 24 h. The mixture was evaporated in vacuo and the residue partitioned between aqueous NaOH (1 M, 1 L) and dichloromethane (3×200 mL). The combined organic extracts were washed with aqueous NaOH (1 M, 500 mL), water (500 mL) and brine (250 mL), then dried (Na2SO4) and evaporated in vacuo to give a solid. Crystallisation from methanol following decolourisation with charcoal gave the title compound (38 g, 61%) as pale yellow needles.

1. temperaturewas heated
2. temperatureat reflux for 24 h
3. customThe mixture was evaporated in vacuo
4. customthe residue partitioned between aqueous NaOH (1 M, 1 L) and dichloromethane (3×200 mL)
5. washThe combined organic extracts were washed with aqueous NaOH (1 M, 500 mL), water (500 mL) and brine (250 mL)
6. dry with materialdried (Na2SO4)
7. customevaporated in vacuo
8. customto give a solid
9. customCrystallisation from methanol following decolourisation with charcoal