反应详情

2-amino-2-(hydroxymethyl)propane-1,3-diol hydrochloride (320 g, 2.03 mol), 2,2-dimethoxypropane (240 g, 2.30 mol), and p-toluenesulfonic acid monohydrate (16.2 g, 102 mmol) were combined into anhydrous dimethylformamide (1.0 L). The solution was stirred vigorously by a mechanical stirrer for 48 hours at room temperature. Triethyl amine (300 mL) and ethyl acetate (1.5 L) were added. A white precipitate formed immediately. The white salt was filtered off and the low boiling point solvents were removed by a rotary evaporator. The product, (5-amino-2,2-dimethyl-1,3-dioxan-5-yl)methanol, was obtained by distillation (250 g, 76%), by 107° C./0.3 torr. 1H NMR (300 MHz, CDCl3) δ1.48 (s, 3H), 1.53 (s, 3H), 3.14 (br, 2H), 3.51 (s, 1H), 3.53 (d, 2H), 3.78 (d, 2H).

1. customA white precipitate formed immediately
2. filtrationThe white salt was filtered off
3. customthe low boiling point solvents were removed by a rotary evaporator