反应详情

温度

27.5 °C

A mixture of 1-(3-hydroxy-phenyl)-propan-1-one (5 g, 0.03 mol), paraformaldehyde (1 g, 0.03 mol), dimethylamine hydrochloride (3 g, 0.04 mol), hydrochloric acid (3.4 ml, 30%) and isopropanol (15 ml) was refluxed for 16 hours. Isopropanol was distilled off from the reaction mixture and resulting reaction mass was cooled to 25-30° C. Water (15 ml) was added to the reaction mass and washed with isopropyl ether (2×15 ml). Layers were separated and aqueous layer was added to a stirred mixture of aqueous sodium hydroxide solution (1.2 g in 16 ml water) and methyl tert-butyl ether (25 ml). Layers were separated. Organic layer was washed with water (10 ml), dried and solvent was distilled to give 3.45 g of the title compound.

1. temperaturewas refluxed for 16 hours
2. distillationIsopropanol was distilled off from the reaction mixture
3. customresulting
4. customreaction mass
5. washwashed with isopropyl ether (2×15 ml)
6. customLayers were separated
7. additionaqueous layer was added to a stirred mixture of aqueous sodium hydroxide solution (1.2 g in 16 ml water) and methyl tert-butyl ether (25 ml)
8. customLayers were separated
9. washOrganic layer was washed with water (10 ml)
10. customdried
11. distillationsolvent was distilled