Dibutylamine → N,N-Dibutyl-3-oxobutanamide

HRID 400204노트

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HRID 400204 반응식
[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]

참가 물질

4

반응물 2

HCID 8148DibutylamineHCID 8868Ethyl Acetoacetate

생성물 1

HCID 243714N,N-Dibutyl-3-oxobutanamide수율 67.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-43ba1776ad0d4475bd7f9e0bb00232af
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05827881

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