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Trifluoroacetic acid → HCID 21912819, 화합물

HRID 1245619
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HRID 1245619 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][CH:18]([C:21]2[C:22]([O:31][CH3:32])=[N:23][N:24]([CH3:30])[C:25]=2[C:26]([F:29])([F:28])[F:27])[CH2:17][CH2:16]1)=O)(C)(C)C>C(Cl)Cl>[CH3:32][O:31][C:22]1[C:21]([CH:18]2[CH2:17][CH2:16][NH:15][CH2:20][CH2:19]2)=[C:25]([C:26]([F:28])([F:27])[F:29])[N:24]([CH3:30])[N:23]=1
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참가 물질

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반응물 2

HCID 6422Trifluoroacetic acidHCID 86592098HCID 86592098, 화합물

생성물 1

HCID 21912819HCID 21912819, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (3.0 mL) was added to a solution of 1-(tert-butoxycarbonyl-4-(3-methoxy-1-methyl-5-(trifluoromethyl)-(1H)-pyrazol-4-yl)piperidine (150 mg, 0.41 mmol, from Step D) in CH2Cl2 (3.0 mL). After 2 h, the reaction was concentrated and the residue was dissolved in EtOAc (15 mL) and washed with saturated aq. NaHCO3 (6 mL) followed by saturated aq. NaCl (5 mL). The organic layer was dried (Na2SO4), decanted, and evaporated to give the title compound as a white solid. For the title compound: 1H NMR (500 MHz, CD3OD) δ 3.89 (s, 3H), 3.80 (s, 3H), 3.32 (d, J=13, 2H), 2.95 (tt, J=13, 4, 1H), 2.93 (td, J=13, 3, 2H), 2.18 (qd, J=13, 4, 2H), 1.76 (d, J=13, 2H); ESI-MS 264.1 (M+H); HPLC A: 1.3 min.

후처리

  1. concentrationthe reaction was concentrated
  2. dissolutionthe residue was dissolved in EtOAc (15 mL)
  3. washwashed with saturated aq. NaHCO3 (6 mL)
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. customdecanted
  6. customevaporated

출처 및 근거

ORD 기록
ord-bf129b50378341f199c1a9e3efef0e17
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07125887B2

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