反应详情

A mixture of 4.6 g (30.6 mmol) of 4-hydroxy 3,5-dimethyl benzaldehyde (Example E), 4.4 g (35 mmol) of benzyl chloride and 4.8 g (35 mmol) of anhydrous potassium carbonate in 100 mL of acetonitrile, is stirred at reflux for 18 hours overnight. The reaction flask and the inorganic salts are washed with fresh acetonitrile and the solvent is removed on a rotary evaporator. A diethyl ether solution of the residue is washed with 2×25 mL of 1N potassium hydroxide solution, brine, dried (magnesium sulfate) and evaporated. Distillation through a short path apparatus affords 6.5 g of the title compound; bp 149°-152° C./0.50 mm (190°-195° C).

1. temperatureat reflux for 18 hours overnight
2. washThe reaction flask and the inorganic salts are washed with fresh acetonitrile
3. customthe solvent is removed on a rotary evaporator
4. washA diethyl ether solution of the residue is washed with 2×25 mL of 1N potassium hydroxide solution, brine
5. dry with materialdried (magnesium sulfate)
6. customevaporated
7. distillationDistillation through a short path apparatus