Acetic Anhydride → Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester

HRID 526152

반응식

HRID 526152 반응식
[C:1]([O:7][CH2:8][CH3:9])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].[CH:10](OCC)(OCC)[O:11][CH2:12][CH3:13].C(OC(=O)C)(=O)C>>[CH2:12]([O:11][CH:10]=[C:2]([C:3](=[O:4])[CH3:5])[C:1]([O:7][CH2:8][CH3:9])=[O:6])[CH3:13]

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 8868Ethyl AcetoacetateHCID 31214Ethyl orthoformate

생성물 1

HCID 97734Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester수율 70%

반응 조건

온도
135 °C

실험 절차

A mixture of ethyl acetoacetate (100 g, 0.77 mol), triethyl orthoformate (130 g, 0.92 mol), and acetic anhydride (150 g, 1.5 mol) was heated at 135° C. for 6-18 h in a round bottomed flask that was equipped with a distillation apparatus to collect the ethanol generated during the reaction. The reaction was cooled, concentrated and the residue was distilled under high vacuum to obtain the desired product (100 g, 70%) as a pale yellow oil: ESI MS m/z 187 [M+H]+.

후처리

  1. customwas equipped with a distillation apparatus
  2. customto collect the ethanol
  3. customgenerated during the reaction
  4. temperatureThe reaction was cooled
  5. concentrationconcentrated
  6. distillationthe residue was distilled under high vacuum

출처 및 근거

ORD 기록
ord-8570c88f10834a9a95744fb4189550c1
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09345709B2

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