HRID839996

反应详情

EQUATION

反应方程式

HRID 839996 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 6 hours. The solution was then allowed to stand overnight, after which 10.0 g of potassium carbonate were added and the methanol was removed by evaporation under reduced pressure. The residue was extracted with benzene, and the benzene extract was washed with water and then dried over potassium carbonate. After removing the benzene, the residue was distilled under reduced pressure, giving 14.0 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 removed by evaporation under reduced pressure
  2. extractionThe residue was extracted with benzene
  3. extractionthe benzene extract
  4. washwas washed with water
  5. dry with materialdried over potassium carbonate
  6. customAfter removing the benzene
  7. distillationthe residue was distilled under reduced pressure