HRID616537

反应详情

EQUATION

反应方程式

HRID 616537 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.3 g of the 5-amino-5-methyl-3-heptanone thus obtained were dissolved in 100 ml of methanol, and 10.0 g of cyclohexanone and 10.0 g of ammonium bromide were added to the resulting solution. Dry ammonia was then introduced into the solution at room temperature for a period of 6 hours. After allowing the solution to stand overnight, 10.0 g of potassium carbonate were added and the methanol was then removed by distillation under reduced pressure. The residue was extracted with benzene, washed with water and dried over potassium carbonate. The benzene was then removed and the residue was distilled under reduced pressure, giving 14.0 g of 2,4-diethyl-4-methyl-1,5-diazaspiro[5.5]-undec-1-ene (bp 93° - 94° C/1.5 mmHg).

WORKUP

后处理

  1. customthe methanol was then removed by distillation under reduced pressure
  2. extractionThe residue was extracted with benzene
  3. washwashed with water
  4. dry with materialdried over potassium carbonate
  5. customThe benzene was then removed
  6. distillationthe residue was distilled under reduced pressure