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

HRID 1772032노트

반응식

HRID 1772032 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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]+.

후처리

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

출처 및 근거

ORD 기록
ord-976468acb9fa4f78aeda526a0803f86f
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09249162B2

반응 노트

불러오는 중…