Hydrochloric Acid → Thieno[2,3-b]pyridine-2,3-diamine HCl salt

HRID 1772032ノート

反応式

HRID 1772032 の反応式
[N+:1]([C:4]1[S:12][C:7]2=[N:8][CH:9]=[CH:10][CH:11]=[C:6]2[C:5]=1[NH2:13])([O-])=O.[ClH:14].CCOC(C)=O>CCO.[Ni]>[ClH:14].[S:12]1[C:7]2=[N:8][CH:9]=[CH:10][CH:11]=[C:6]2[C:5]([NH2:13])=[C:4]1[NH2:1]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 131693742-Nitrothieno[2,3-b]pyridin-3-amine

生成物 1

HCID 68089372Thieno[2,3-b]pyridine-2,3-diamine HCl salt

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

To a suspension of 2-nitrothieno[2,3-b]pyridin-3-amine (1.1 g, 5.6 mmol) in EtOH (60 mL) was added Raney Ni (1 g), followed by slow addition of N2H4.H2O (1.4 g, 22 mmol). The mixture was stirred at room temperature for 2 h. A solution of HCl in EtOAc (1 M, 18 mL, 18 mmol) was added to the reaction mixture slowly, and the mixture was filtered. The filter cake was washed with EtOAc (20 mL×3), then dried under reduced pressure to give the crude product as a yellow solid (2.7 g). ESI MS: m/z 166 [M+H]+.

後処理

  1. filtrationthe mixture was filtered
  2. washThe filter cake was washed with EtOAc (20 mL×3)
  3. customdried under reduced pressure

出典と根拠

ORDレコード
ord-976468acb9fa4f78aeda526a0803f86f
出典データセット
uspto-grants-2016_02
特許番号
US09249162B2

反応ノート

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