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

HRID 1258680노트

반응식

HRID 1258680 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fd56f015cb654c11a4748a557d730aa6
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466186B2

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