Hydrochloric Acid → (1-cyclohexyl-2-(5-(3-(methoxymethyl)phenyl)-1H-indazol-3-ylamino)-1H-benzo[d]imidazol-5-yl)methanol

HRID 2068293ノート

反応式

HRID 2068293 の反応式
[CH:1]1([N:7]2[C:11]3[CH:12]=[CH:13][C:14]([CH2:16][OH:17])=[CH:15][C:10]=3[N:9]=[C:8]2[NH:18][C:19]2[C:27]3[C:22](=[CH:23][CH:24]=[C:25]([C:28]4[CH:33]=[CH:32][CH:31]=[C:30]([CH2:34][O:35][CH3:36])[CH:29]=4)[CH:26]=3)[N:21](COCC[Si](C)(C)C)[N:20]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl>C(O)C>[CH:1]1([N:7]2[C:11]3[CH:12]=[CH:13][C:14]([CH2:16][OH:17])=[CH:15][C:10]=3[N:9]=[C:8]2[NH:18][C:19]2[C:27]3[C:22](=[CH:23][CH:24]=[C:25]([C:28]4[CH:33]=[CH:32][CH:31]=[C:30]([CH2:34][O:35][CH3:36])[CH:29]=4)[CH:26]=3)[NH:21][N:20]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67253467(1-cyclohexyl-2-(5-(3-(methoxymethyl)phenyl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazol-3-ylamino)-1H-benzo[d]imidazol-5-yl)methanol

生成物 1

HCID 24798548(1-cyclohexyl-2-(5-(3-(methoxymethyl)phenyl)-1H-indazol-3-ylamino)-1H-benzo[d]imidazol-5-yl)methanol収率 26%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In a 20 mL vial with septum cover was added {1-cyclohexyl-2-[5-(3-methoxymethyl-phenyl)-1-(2-trimethylsilanyl-ethoxymethyl)-1H-indazol-3-ylamino]-1H-benzoimidazol-5-yl}-methanol (58 mg, 0.000095 mol), ethanol (6.0 mL) and HCl (2.0 mL, 0.065 M). The mixture was refluxed for 1.5 hr. The mixture was concentrated and the residue dissolved in approx 1.5 mL of DMSO and purified by HPLC. The product fractions were lyopholized overnight to give 11.9 mg of the title compound as an off white solid.

後処理

  1. temperatureThe mixture was refluxed for 1.5 hr
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue dissolved in approx 1.5 mL of DMSO
  4. custompurified by HPLC

出典と根拠

ORDレコード
ord-67d30d8955f643ebac3a69e0afba5200
出典データセット
uspto-grants-2012_10
特許番号
US08293923B2

反応ノート

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