反应详情

A solution of laevulinic acid (50 g, 0.43 mol) in water (200 ml) was added to a mixture of 3,4,5-trimethoxybenzaldehyde (85 g, 0.43 mol) in ethanol (150 ml) and sodium hydroxide solution (5%, 700 ml). The mixture was warmed with vigorous stirring until all the aldehyde had dissolved and was then poured onto ice (ca 2 Kg). It was then acidified to pH3-4 and left overnight. The crystalline material formed was filtered off, dried in vacuo and then recrystallised from ethanol to give pale yellow crystals (30.08 g), m.p. 187°-9°.

1. temperatureThe mixture was warmed
2. dissolutionhad dissolved
3. additionwas then poured onto ice (ca 2 Kg)
4. customThe crystalline material formed
5. filtrationwas filtered off
6. customdried in vacuo
7. customrecrystallised from ethanol