反应详情

To a solution of 7.6 grams (0.05 mole) of 2',6'-dihydroxyacetophenone and 6.1 gram (0.05 mole) p-hydroxybenzaldehyde in ethanol was added 100 ml. of 60% aqueous sodium hydroxide. The mixture was stirred at room temperature for 18 hours and then acidified with 6 N hydrochloric acid. The resulting orange solid was collected by filtration and washed with water. The solid was chromatographed on silica gel (200 g., 2.25 l., 20% acetone-Skellysolve "B") and 150 ml. fractions taken. Fractions 6-12 were combined and crystallized from methanol-methylene chloride giving fine orange needles, 28 g., m.p. 190°-192° C., resolidified and melted 210°-212° C., 22% yield).

1. filtrationThe resulting orange solid was collected by filtration
2. washwashed with water
3. customThe solid was chromatographed on silica gel (200 g., 2.25 l., 20% acetone-Skellysolve "B") and 150 ml
4. customcrystallized from methanol-methylene chloride giving fine orange needles, 28 g
5. custommelted 210°-212° C.