Hydrofluoric Acid → HCID 178523815、化合物

HRID 1690594ノート

反応式

HRID 1690594 の反応式
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

参加物

5

反応物 2

HCID 14917Hydrofluoric AcidHCID 178455367HCID 178455367、化合物

生成物 1

HCID 178523815HCID 178523815、化合物収率 25%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 131729614iPrOAc brine溶媒

実験手順

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+].

後処理

  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

出典と根拠

ORDレコード
ord-f98419bd2304450e8c3d8ae65fdaf8f7
出典データセット
uspto-grants-2012_04
特許番号
US08153663B2

反応ノート

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