反应详情

1,2,4-triacetoxybenzene (6.3 g, 25 mmol) and ethyl 2-benzylacetoacetate (5.5 g, 25 mmol) were heated together as described in Example 1. 75% sulphuric acid (35 ml) was added to the stirred solution and stirring continued for 16 hours. The dark coloured suspension was poured into ice/water (350 ml) with good stirring and the grey suspension filtered and the residue washed with abundant water. The residual solid was air dried and recrystallised from hot ethanol with subsequent addition of a little water to aid crystallisation. The esculetin derivative formed small white needles (5.5 g, 75.3%).

1. stirringwith good stirring
2. filtrationthe grey suspension filtered
3. washthe residue washed with abundant water
4. customdried
5. customrecrystallised from hot ethanol with subsequent addition of a little water
6. customcrystallisation