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Trifluoroacetic acid → 3-(4-Trifluoromethyl-phenyl)-2,5-dihydro-1H-pyrrole

HRID 552679
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인쇄 미리보기

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HRID 552679 반응식
[F:1][C:2]([F:16])([F:15])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2(O)[CH2:13][CH2:12][NH:11][CH2:10]2)=[CH:5][CH:4]=1.C(O)(C(F)(F)F)=O>ClCCl>[F:16][C:2]([F:1])([F:15])[C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH2:10][NH:11][CH2:12][CH:13]=2)=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 1208963-(4-(Trifluoromethyl)phenyl)pyrrolidin-3-ol

생성물 1

HCID 590304773-(4-Trifluoromethyl-phenyl)-2,5-dihydro-1H-pyrrole수율 18%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a suspension of 0.43 mmol rac-3-(4-Trifluoromethyl-phenyl)-pyrrolidin-3-ol in 0.4 ml dichloromethane under argon, was added 0.4 ml TFA. The reaction mixture was stirred at reflux for 5 days and concentrated. The residue was dissolved in ethyl acetate and NaOH 2N was added until pH 9-10. The organic phases were dried over Na2SO4 and evaporated to yield the title compound (18%) as an oil MS (m/e): 214.2 ([M+1], 100%).

후처리

  1. temperatureat reflux for 5 days
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. additionNaOH 2N was added until pH 9-10
  5. dry with materialThe organic phases were dried over Na2SO4
  6. customevaporated

출처 및 근거

ORD 기록
ord-62bb67eed92d497d9672300223e300d4
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07951836B2

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