反应详情

To a 500 mL flask containing 1-amino-cyclohexylmethanol (135 g, 1.05 mol) and methanol (50 mL) is added methyl formcel (53 mL of 55% formaldehyde in methanol/water, 1.06 mol) dropwise over a 1 hour period. During the addition, the stirred solution is warmed gently from room temperature to 37° C. After the addition is completed, the mixture is allowed to stir overnight at room temperature. The clear, colorless reaction mixture is stripped on a rotary evaporator (50° C./29″ vacuum). The resulting oil is distilled under vacuum giving a clear, colorless, mobile liquid with a boiling point of 43° C./0.8 torr. A total of 123.4 g is collected (83% yield). A GC analysis indicates 95.6% purity.

1. additionDuring the addition
2. temperaturethe stirred solution is warmed gently from room temperature to 37° C
3. additionAfter the addition
4. customThe clear, colorless reaction mixture is stripped on a rotary evaporator (50° C./29″ vacuum)
5. distillationThe resulting oil is distilled under vacuum
6. customgiving a clear, colorless, mobile liquid with a boiling point of 43° C./0.8 torr
7. customA total of 123.4 g is collected (83% yield)