反应 #944022

ord-b1f4b954edb34e5c9a6451808d73c45e

反应方程式

CCCC=O
butyraldehyde
CC(C)NC(C)C
diisopropylamine
CCC=CN(C(C)C)C(C)C
title compound
收率 65.0%
CCC=CN(C(C)C)C(C)C
1-(N,N-Diisopropylamino)-1-butene
收率 65.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture was heated
  2. 2
    温度under reflux
  3. 3
    其他while removing the water
  4. 4
    其他produced, until the production of water
  5. 5
    其他(about 15 hours)
  6. 6
    其他The solvent was then removed by distillation under reduced pressure
  7. 7
    workup.DISTILLATIONthe residue was distilled under atmospheric pressure
  8. 8
    其他of from 140 to 160° C.
  9. 9
    其他were collected

实验过程

6.25 ml (69.3 mmol) of butyraldehyde and 19.44 ml (139 mmol) of diisopropylamine were dissolved in 30 ml of benzene, and the mixture was heated under reflux, while removing the water produced, until the production of water stopped (about 15 hours). The solvent was then removed by distillation under reduced pressure, and the residue was distilled under atmospheric pressure. Those fractions of the distillate having a boiling point of from 140 to 160° C. were collected, to give 6.95 g of the title compound as a pale yellow oily substance (yield 65%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE039420E1uspto-grants-2006_12