Trifluoroacetic acid → (E)-3-[5-(1H-imidazol-1-yl)-6-methoxypyridin-2-yl]acrylic acid

HRID 546788노트

반응식

HRID 546788 반응식
FC(F)(F)C(O)=O.[N:8]1([C:13]2[CH:14]=[CH:15][C:16](/[CH:21]=[CH:22]/[C:23]([O:25]C(C)(C)C)=[O:24])=[N:17][C:18]=2[O:19][CH3:20])[CH:12]=[CH:11][N:10]=[CH:9]1>ClCCl>[N:8]1([C:13]2[CH:14]=[CH:15][C:16](/[CH:21]=[CH:22]/[C:23]([OH:25])=[O:24])=[N:17][C:18]=2[O:19][CH3:20])[CH:12]=[CH:11][N:10]=[CH:9]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66839426tert-butyl (E)-3-[5-(1H-imidazol-1-yl)-6-methoxypyridin-2-yl]acrylate

생성물 1

HCID 66839409(E)-3-[5-(1H-imidazol-1-yl)-6-methoxypyridin-2-yl]acrylic acid수율 86.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of trifluoroacetic acid (3 mL) in dichloromethane (1.5 mL) was added to tert-butyl (E)-3-[5-(1H-imidazol-1-yl)-6-methoxypyridin-2-yl]acrylate (490 mg) under ice-cooling, and the reaction solution was stirred at room temperature for one hour. The reaction solution was concentrated under reduced pressure, diluted with chloroform and then concentrated under reduced pressure. Diethyl ether was added to the residue, and the precipitated solid was collected by filtration. The solid was washed with diethyl ether to obtain the title compound as a solid (345 mg). The property values of the compound are as follows.

후처리

  1. temperaturecooling
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additiondiluted with chloroform
  4. concentrationconcentrated under reduced pressure
  5. additionDiethyl ether was added to the residue
  6. filtrationthe precipitated solid was collected by filtration
  7. washThe solid was washed with diethyl ether

출처 및 근거

ORD 기록
ord-de91bd2631ce41aa911c5c7cddf9b522
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935815B2

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