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Trifluoroacetic acid → 3-Chloro-4-{[3-(4-chlorophenyl)-4-cyclopropyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]methyl}benzoic acid

HRID 536546
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HRID 536546 반응식
C([O:5][C:6](=[O:31])[C:7]1[CH:12]=[CH:11][C:10]([CH2:13][N:14]2[C:18](=[O:19])[N:17]([CH:20]3[CH2:22][CH2:21]3)[C:16]([C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=3)=[N:15]2)=[C:9]([Cl:30])[CH:8]=1)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:30][C:9]1[CH:8]=[C:7]([CH:12]=[CH:11][C:10]=1[CH2:13][N:14]1[C:18](=[O:19])[N:17]([CH:20]2[CH2:22][CH2:21]2)[C:16]([C:23]2[CH:24]=[CH:25][C:26]([Cl:29])=[CH:27][CH:28]=2)=[N:15]1)[C:6]([OH:31])=[O:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 58460119tert-Butyl-3-chloro-4-{[3-(4-chlorophenyl)-4-cyclopropyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]methyl}benzoate

생성물 1

HCID 584601203-Chloro-4-{[3-(4-chlorophenyl)-4-cyclopropyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]methyl}benzoic acid

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

An amount of 1.38 g (3.00 mmol) of the compound from Example 26A was dissolved in 10 ml of dichloromethane and admixed at RT with 3.0 ml (39 mmol) of trifluoroacetic acid and stirred at RT for 72 h. The mixture was concentrated under reduced pressure and admixed with 10 ml of toluene and concentrated again. This procedure was repeated a further two times. The residue which remained was freed from remnants of solvent under a high vacuum. This gave 1.27 g (63% of theory) of the target compound with a purity of 60%.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. concentrationconcentrated again

출처 및 근거

ORD 기록
ord-33b0938a1d144cd4bf258c2f4d6b00b9
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859601B2

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