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Trifluoroacetic acid → HCID 11720107, 화합물

HRID 2054173
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HRID 2054173 반응식
C(O[N:6]([CH2:10][C:11]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[C:16]([CH:21]2[CH2:26][CH2:25][N:24]([CH2:27][C:28]3[CH:33]=[CH:32][C:31]([S:34][C:35]4[CH:40]=[CH:39][C:38]([O:41][CH3:42])=[CH:37][CH:36]=4)=[CH:30][CH:29]=3)[CH2:23][CH2:22]2)[CH:15]=1)=[O:12])[C:7](C)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl.C([O-])(O)=O.[Na+]>[CH3:42][O:41][C:38]1[CH:39]=[CH:40][C:35]([S:34][C:31]2[CH:30]=[CH:29][C:28]([CH2:27][N:24]3[CH2:25][CH2:26][CH:21]([C:16]4[CH:15]=[C:14]([NH:13][C:11](=[O:12])[CH2:10][NH:6][CH3:7])[CH:19]=[CH:18][C:17]=4[CH3:20])[CH2:22][CH2:23]3)=[CH:33][CH:32]=2)=[CH:36][CH:37]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 86604273HCID 86604273, 화합물

생성물 1

HCID 11720107HCID 11720107, 화합물수율 99.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 516892Sodium Bicarbonate용매

실험 절차

2-[(tert-butoxy)-N-methylcarbonylamino]-N-[3-(1-{[4-(4-methoxyphenylthio)phenyl]methyl} (4-piperidyl))-4-methylphenyl]acetamide was dissolved in CH2Cl2 (1.00 mL) and trifluoroacetic acid (0.160 mL) was added to the stirred solution. Stirring was continued for 10 min then the reaction mixture was concentrated in vacuo to give a gum. The crude product was dissolved in saturated NaHCO3 solution (10 mL to pH 10) and extracted with CH2Cl2 (2×10 mL). The combined organic layers were dried over MgSO4 and concentrated in vacuo to give N-[3-(1-{[4-(4-methoxyphenylthio)phenyl]methyl}(4-piperidyl))-4-methylphenyl]2-(methylamino)acetamide (68.6 mg, 99.2% yield) as a yellow solid.

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customto give a gum
  3. extractionextracted with CH2Cl2 (2×10 mL)
  4. dry with materialThe combined organic layers were dried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-8a2927c8e01e43a1bbcb07fe2b1bbafa
출처 데이터셋
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07329656B2

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