Hydrochloric Acid → 2,4-Dichloro-3-[5-chloro-1-methyl-6-(3-(trifluoromethyl)piperidin-1-yl)-1H-benzimidazol-2-ylamino]benzylamine

HRID 1258680ノート

反応式

HRID 1258680 の反応式
Cl.C(OC(=O)[NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[C:12]([NH:17][C:18]2[N:22]([CH3:23])[C:21]3[CH:24]=[C:25]([N:29]4[CH2:34][CH2:33][CH2:32][CH:31]([C:35]([F:38])([F:37])[F:36])[CH2:30]4)[C:26]([Cl:28])=[CH:27][C:20]=3[N:19]=2)[C:11]=1[Cl:39])(C)(C)C>O1CCOCC1>[Cl:39][C:11]1[C:12]([NH:17][C:18]2[N:22]([CH3:23])[C:21]3[CH:24]=[C:25]([N:29]4[CH2:34][CH2:33][CH2:32][CH:31]([C:35]([F:38])([F:37])[F:36])[CH2:30]4)[C:26]([Cl:28])=[CH:27][C:20]=3[N:19]=2)=[C:13]([Cl:16])[CH:14]=[CH:15][C:10]=1[CH2:9][NH2:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86674334N-{2,4-Dichloro-3-[5-chloro-1-methyl-6-(3-(trifluoromethyl)piperidin-1-yl)-1H-benzimidazol-2-ylamino]benzyl}-carbamic acid tert-butyl ester

生成物 1

HCID 866743352,4-Dichloro-3-[5-chloro-1-methyl-6-(3-(trifluoromethyl)piperidin-1-yl)-1H-benzimidazol-2-ylamino]benzylamine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

4 M HCl in dioxane (38 mL) was added to N-{2,4-dichloro-3-[5-chloro-1-methyl-6-(3-(trifluoromethyl)piperidin-1-yl)-1H-benzimidazol-2-ylamino]benzyl}-carbamic acid tert-butyl ester (5.4 g, 8.9 mmol) in dioxane (300 mL) and stirred at rt overnight. The reaction mixture was concentrated and the resulting residue was diluted with aq. NaHCO3-solution. The aq. phase was extracted with EtOAc, the organic phase was dried with Na2SO4 and concentrated.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionthe resulting residue was diluted with aq. NaHCO3-solution
  3. extractionThe aq. phase was extracted with EtOAc
  4. dry with materialthe organic phase was dried with Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-fd56f015cb654c11a4748a557d730aa6
出典データセット
uspto-grants-2013_06
特許番号
US08466186B2

反応ノート

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