HRID465152

反应详情

EQUATION

反应方程式

HRID 465152 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

31.8 g (0.30 mol) of sodium acetylcyanamide are dissolved in 75 ml of dimethylformamide at 100° C., and 36.9 g (0.30 mol) of isopropyl bromide are added dropwise in the course of 11/2 hours. The mixture is allowed to afterreact at 100° C. for 3 hours, and then 200 ml of acetone are added and the NaBr which has precipitated is filtered off with suction (28.2 g=0.27 mol). The acetone is then removed on a rotary evaporator and the residue is distilled under a waterpump vacuum in order to isolate all the distillable constituents. Fractional distillation of this distillate over a spinning bank column give 14.3 g (37.8% of theory) of a product of boiling point 107° C./90 mbar which, according to gas chromatography, is a single product.

WORKUP

后处理

  1. customthe NaBr which has precipitated
  2. filtrationis filtered off with suction (28.2 g=0.27 mol)
  3. customThe acetone is then removed on a rotary evaporator
  4. distillationthe residue is distilled under a waterpump vacuum in order
  5. customto isolate all the distillable constituents
  6. distillationFractional distillation of this distillate over a spinning bank column
  7. customgive 14.3 g (37.8% of theory) of a product of boiling point 107° C./90 mbar which