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Acetic Anhydride → Ethyl 3-ethoxy-2-(2,4,5-trifluoro-3-methoxybenzoyl)acrylate

HRID 1770109
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인쇄 미리보기

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HRID 1770109 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][C:6](=[O:18])[C:7]1[CH:12]=[C:11]([F:13])[C:10]([F:14])=[C:9]([O:15][CH3:16])[C:8]=1[F:17])[CH3:2].[CH:20]([O-])([O-])[O:21][CH2:22][CH3:23].C(OC(=O)C)(=O)C>>[CH3:16][O:15][C:9]1[C:8]([F:17])=[C:7]([CH:12]=[C:11]([F:13])[C:10]=1[F:14])[C:6]([C:5](=[CH:20][O:21][CH2:22][CH3:23])[C:4]([O:3][CH2:1][CH3:2])=[O:19])=[O:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 10588473Ethyl 3-oxo-3-(2,4,5-trifluoro-3-methoxyphenyl)propanoateHCID 53630039Ethylorthoformate

생성물 1

HCID 54548840Ethyl 3-ethoxy-2-(2,4,5-trifluoro-3-methoxybenzoyl)acrylate수율 98.6%

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온도
110 °C

실험 절차

A mixture of ethyl-3-methoxy-2,4,5-trifluorobenzoylacetate (500 mg, 1.8 mmol), ethyl orthoformate (0.45 mL, 2.72 mmol) and acetic anhydride (460 mg, 4.5 mmol, 2.5 eq) was stirred at 110° C. for 12 hours and the excess reagents were removed by distillation under high vacuum (0.1 mmHg) to give 590 mg of a yellow-orange oil. This material was used directly in the next step without further purification or characterization.

후처리

  1. customthe excess reagents were removed by distillation under high vacuum (0.1 mmHg)

출처 및 근거

ORD 기록
ord-3ee6a5d6d6b74eb58ddc853776f7a5b1
출처 데이터셋
uspto-grants-1995_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05385913

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