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 410120ノート

反応式

HRID 410120 の反応式
[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]

参加物

4

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bac7058a157a4625a581e78e28f76c3d
出典データセット
uspto-grants-2014_06
特許番号
US08759537B2

反応ノート

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