反应详情

To a solution of 2,6-bis(hydroxymethyl)-p-cresol (1) (250 g, 1.48 mol), NaOH pellet (90 g, 2.25 mol) in water (2 L), dimethyl sulfate (105 g, 0.84 mol) was added slowly while stirring. The temperature of the reaction mixture was maintained below 40° C. during dimethyl sulfate addition. Copious white precipitate formed upon standing overnight, the white product (150 g) was collected by filtration as the first crop. Dimethyl sulfate (31 g, 0.25 mol) was added to the mother liquor, and the mixture was stirred at room temperature for 5 days. During this time the volume of the mother liquor was reduced to half of its original volume and 70 g of product was collected as the second crop by filtration. Total yield, 220 g (81%).

1. customCopious white precipitate formed
2. filtrationthe white product (150 g) was collected by filtration as the first crop
3. stirringthe mixture was stirred at room temperature for 5 days
4. filtrationwas collected as the second crop by filtration