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Trifluoroacetic acid → 5-Methyl-2-[4-(piperidin-4-yloxy)phenyl]-2H-pyrazole-3-carboxylic acid cyclohexylamide

HRID 1013035
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HRID 1013035 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([N:21]3[C:25]([C:26](=[O:34])[NH:27][CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)=[CH:24][C:23]([CH3:35])=[N:22]3)=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[CH:28]1([NH:27][C:26]([C:25]2[N:21]([C:18]3[CH:17]=[CH:16][C:15]([O:14][CH:11]4[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]4)=[CH:20][CH:19]=3)[N:22]=[C:23]([CH3:35])[CH:24]=2)=[O:34])[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33]1
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참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 589487744-[4-(5-Cyclohexylcarbamoyl-3-methylpyrazol-1-yl)phenoxy]piperidine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 589487705-Methyl-2-[4-(piperidin-4-yloxy)phenyl]-2H-pyrazole-3-carboxylic acid cyclohexylamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-[4-(5-cyclohexylcarbamoyl-3-methylpyrazol-1-yl)phenoxy]piperidine-1-carboxylic acid tert-butyl ester (482 mg, 1.00 mmol) in methylene chloride (10 mL) was added trifluoroacetic acid (2 mL). After the reaction was stirred at room temperature for 2 hours, it was quenched with saturated sodium bicarbonate and the aqueous layer was extracted with methylene chloride. The combined organic layers were dried (MgSO4) and concentrated to give the crude product in quantitative yield. LC-MS (C22H30N4O2 calculated 382) m/z 383 (M+H).

후처리

  1. customit was quenched with saturated sodium bicarbonate
  2. extractionthe aqueous layer was extracted with methylene chloride
  3. dry with materialThe combined organic layers were dried (MgSO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e547fd2845ed477abcc09f135fdee842
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07981896B2

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