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Acetic Anhydride → 2-(2-Ethyl-butyryl)-3-ethoxy-but-2-enenitrile

HRID 324374
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HRID 324374 반응식
[CH2:1]([CH:3]([CH2:9][CH3:10])[C:4](=[O:8])[CH2:5][C:6]#[N:7])[CH3:2].[C:11]([O:14][C:15](=O)[CH3:16])(=O)[CH3:12].C(OCC)(OCC)(OCC)C>C(OCC)(=O)C.O>[CH2:1]([CH:3]([CH2:9][CH3:10])[C:4]([C:5](=[C:11]([O:14][CH2:15][CH3:16])[CH3:12])[C:6]#[N:7])=[O:8])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 66221Triethyl orthoacetateHCID 235057484-Ethyl-3-oxohexanenitrile

생성물 1

HCID 540497052-(2-Ethyl-butyryl)-3-ethoxy-but-2-enenitrile

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

A mixture of 4-ethyl-3-oxo-hexanenitrile (1.013 g, 7.28 mmol), acetic anhydride (1.5 ml) and triethyl orthoacetate (1.240 g, 7.64 mmol) was heated to reflux overnight. The reaction mixture was taken up in ethyl acetate and water. The brine and the ethyl acetate layer were separated. The organic layer was dried and concentrated to give 1.262 g of dry oil which was used directly for the next reaction. 1H NMR (CDCl3): 0.8-1.0(m,6H), 1.44(t,3H), 1.4-1.8(m,4H), 2.61(s,3H), 3.03(m,1H), 4.28(q, 2H)ppm.

후처리

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. customThe brine and the ethyl acetate layer were separated
  4. customThe organic layer was dried
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b47ea97e79fb4d2b90c1f65e63cfc237
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218397B1

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