HRID465154

反应详情

EQUATION

反应方程式

HRID 465154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

36.0 g (0.20 mol) of 1-bromoheptane are added dropwise to a solution of 21.2 g (0.20 mol) of sodium acetylcyanamide in 50 ml of dimethylformamide at 85° C. The mixture is allowed to after-react for 2 hours and the NaBr is filtered off with suction at room temperature. The filtrate is treated with 50 ml of H2O and the mixture is extracted with cloroform. The solvent is separated off on a rotary evaporator and the crude product is distilled over a rotating belt column to give 24.3 g (66.7% of theory) of pure product of boiling point 124° C./18 mbar.

WORKUP

后处理

  1. customto after-react for 2 hours
  2. filtrationthe NaBr is filtered off with suction at room temperature
  3. additionThe filtrate is treated with 50 ml of H2O
  4. extractionthe mixture is extracted with cloroform
  5. customThe solvent is separated off on a rotary evaporator
  6. distillationthe crude product is distilled over a rotating belt column
  7. customto give 24.3 g (66.7% of theory) of pure product of boiling point 124° C./18 mbar