Hydrochloric Acid → N-(3-Chloro-4-fluoro-phenyl)-2-(2,6-dichloro-3-aminomethyl-phenylamino)-6-(2,2-difluoroethoxy)-1-methyl-1H-benzimidazole-5-carboxylic acid amide

HRID 410120노트

반응식

HRID 410120 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]([C:12]2[C:39]([O:40][CH2:41][CH:42]([F:44])[F:43])=[CH:38][C:15]3[N:16]([CH3:37])[C:17]([NH:19][C:20]4[C:25]([Cl:26])=[CH:24][CH:23]=[C:22]([CH2:27][NH:28]C(OC(C)(C)C)=O)[C:21]=4[Cl:36])=[N:18][C:14]=3[CH:13]=2)=[O:11])[CH:5]=[CH:6][C:7]=1[F:8].Cl>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]([C:12]2[C:39]([O:40][CH2:41][CH:42]([F:43])[F:44])=[CH:38][C:15]3[N:16]([CH3:37])[C:17]([NH:19][C:20]4[C:25]([Cl:26])=[CH:24][CH:23]=[C:22]([CH2:27][NH2:28])[C:21]=4[Cl:36])=[N:18][C:14]=3[CH:13]=2)=[O:11])[CH:5]=[CH:6][C:7]=1[F:8]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 56840392N-(3-chloro-4-fluoro-phenyl)-2-{2,6-dichloro-3-[(tert-butoxy-carbonylamino)-methyl]phenylamino}-6-(2,2-difluoroethoxy)-1-methyl-1H-benzimidazole-5-carboxylic acid amide

생성물 1

HCID 86669639N-(3-Chloro-4-fluoro-phenyl)-2-(2,6-dichloro-3-aminomethyl-phenylamino)-6-(2,2-difluoroethoxy)-1-methyl-1H-benzimidazole-5-carboxylic acid amide

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A mixture of N-(3-chloro-4-fluoro-phenyl)-2-{2,6-dichloro-3-[(tert-butoxy-carbonylamino)-methyl]phenylamino}-6-(2,2-difluoroethoxy)-1-methyl-1H-benzimidazole-5-carboxylic acid amide (4.0 g, 5.9 mmol, prepared in analogy to example 75 from N-(3-chloro-4-fluorophenyl)-2-(2,2-difluoroethoxy)-4-methylamino-5-amino-benzamide with building block B), 4 M HCl in dioxane (50 mL) and dioxane (200 mL) is stirred for 2 h. The precipitate is filtered off, washed with water and diluted with 10 mL conc. aq. NH3. The mixture is extracted with EtOAc, the organic phase is dried with Na2SO4 and concentrated.

후처리

  1. filtrationThe precipitate is filtered off
  2. washwashed with water
  3. additiondiluted with 10 mL conc. aq. NH3
  4. extractionThe mixture is extracted with EtOAc
  5. dry with materialthe organic phase is dried with Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-bac7058a157a4625a581e78e28f76c3d
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759537B2

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