Hydrofluoric Acid → HCID 178523815, 화합물

HRID 1690594노트

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HRID 1690594 반응식
F.C([Si](C)(C)[O:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([NH:14][C:15](=[O:40])[N:16]([C:33]2[CH:38]=[CH:37][CH:36]=[C:35]([Cl:39])[CH:34]=2)[C:17]2[N:18]([C:26]3[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=3)[N:19]=[C:20]3[C:25]=2[CH:24]=[CH:23][CH:22]=[CH:21]3)[CH2:10][CH2:9]1)(C)(C)C>C(OC(C)=O)(C)C.[Cl-].[Na+].O.C(Cl)Cl>[Cl:39][C:35]1[CH:34]=[C:33]([N:16]([C:17]2[N:18]([C:26]3[CH:27]=[CH:28][C:29]([Cl:32])=[CH:30][CH:31]=3)[N:19]=[C:20]3[C:25]=2[CH:24]=[CH:23][CH:22]=[CH:21]3)[C:15]([NH:14][C@H:11]2[CH2:10][CH2:9][C@H:8]([OH:7])[CH2:13][CH2:12]2)=[O:40])[CH:38]=[CH:37][CH:36]=1

참가 물질

5

반응물 2

HCID 14917Hydrofluoric AcidHCID 178455367HCID 178455367, 화합물

생성물 1

HCID 178523815HCID 178523815, 화합물수율 25%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 131729614iPrOAc brine용매

실험 절차

Hydrofluoric acid (48%, 200 μl, 16 μmol) was added to a solution of trans-3-[4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-1-(3-chloro-phenyl)-1-[2-(4-chloro-phenyl)-2H-indazol-3-yl]-urea (10 mg, 16 μmol) in CH3CN/CH2Cl2 1/1 (400 μl). The reaction mixture was stirred for 4 h at ambient temperature, diluted with CH2Cl2 (5 ml) and washed with saturated aqueous NaHCO3 solution and brine. The organic layer was dried over Na2SO4. The solvent was removed under reduced pressure to give the title compound (2 mg, 4 μmol; 25%) as brown solid. MS: m/e=495.5 [M+H+].

후처리

  1. washwashed with saturated aqueous NaHCO3 solution and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-f98419bd2304450e8c3d8ae65fdaf8f7
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08153663B2

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