Dibutylamine → N,N-Dibutyl-3-oxobutanamide

HRID 400204ノート

反応式

HRID 400204 の反応式
[C:1]([O:7]CC)(=O)[CH2:2][C:3]([CH3:5])=[O:4].[CH2:10]([NH:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:11][CH2:12][CH3:13]>C(OCC)C>[CH2:10]([N:14]([CH2:15][CH2:16][CH2:17][CH3:18])[C:1](=[O:7])[CH2:2][C:3](=[O:4])[CH3:5])[CH2:11][CH2:12][CH3:13]

参加物

4

反応物 2

HCID 8148DibutylamineHCID 8868Ethyl Acetoacetate

生成物 1

HCID 243714N,N-Dibutyl-3-oxobutanamide収率 67.7%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
150 °C

実験手順

A! A mixture of ethyl acetoacetate (50 g, 0.38 mole) and dibutylamine (49.65 g, 0.38 mole) was heated to 150° C. for one day. After cooling, the reaction mixture was taken up in 500 ml of ethyl ether and washed with 200 ml of 1N HCl and 200 ml of water. The ether phase was anhydrified over sodium sulfate, and evaporated to dryness thus yielding 86.7 g of a crude which was distilled under vacuum to give 54.86 g (yield: 67%) of N,N-dibutyl-3-oxo-butanamide.

後処理

  1. temperatureAfter cooling
  2. washwashed with 200 ml of 1N HCl and 200 ml of water
  3. customevaporated to dryness
  4. customthus yielding 86.7 g of a crude which
  5. distillationwas distilled under vacuum

出典と根拠

ORDレコード
ord-43ba1776ad0d4475bd7f9e0bb00232af
出典データセット
uspto-grants-1998_10
特許番号
US05827881

反応ノート

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