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Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → Ethyl 3-(2-fluoro-5-methoxyphenyl)acrylate

HRID 709699
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인쇄 미리보기

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HRID 709699 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=O.C1(P(=[CH:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[CH:31][C:32]([O:34][CH2:35][CH3:36])=[O:33]
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참가 물질

4

반응물 2

HCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 27348722-Fluoro-5-methoxybenzaldehyde

생성물 1

HCID 77260531Ethyl 3-(2-fluoro-5-methoxyphenyl)acrylate수율 38.5%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
70 °C

실험 절차

To a solution of 2-fluoro-5-methoxybenzaldehyde (1.54 g) in toluene (50 mL) was added ethyl (triphenylphosphoranylidene)acetate (3.83 g), and the mixture was stirred at 70° C. for 15 hr. The reaction mixture was concentrated, and diethyl ether was added. The insoluble material was filtered off, and the filtrate was concentrated. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (862 mg) as a colorless oil.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additiondiethyl ether was added
  3. filtrationThe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-f6dfcdb008d34d4496d69fd0a6db49d4
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181186B2

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