Ammonium Chloride → HCID 67974925, 화합물

HRID 706655노트

반응식

HRID 706655 반응식
[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH2:10][N:11]2[C:19]3[C:14](=[C:15]([N+:20]([O-])=O)[CH:16]=[CH:17][CH:18]=3)[C:13]([CH3:23])=[N:12]2)[CH:7]=[CH:6][CH:5]=1)[CH3:2].[Cl-].[NH4+]>[Fe].CCO.O>[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH2:10][N:11]2[C:19]3[CH:18]=[CH:17][CH:16]=[C:15]([NH2:20])[C:14]=3[C:13]([CH3:23])=[N:12]2)[CH:7]=[CH:6][CH:5]=1)[CH3:2]

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 67976364HCID 67976364, 화합물

생성물 1

HCID 67974925HCID 67974925, 화합물수율 71.2%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 19096565Water ethanol용매

실험 절차

A solution of 1-((6-ethoxypyridin-2-yl)methyl)-3-methyl-4-nitro-1H-indazole (0.118 g, 0.378 mmol), ammonium chloride (0.0101 g, 0.189 mmol) in 4:1 EtOH/water (2 mL) was treated with iron (0.211 g, 3.78 mmol) and refluxed for 2 hours. The solvent was removed and the residue taken in EtOAc-water and filtered through glass fiber filter paper. The organic phase was separated, dried (phase separator silicone treated filter paper), and concentrated to provide 1-((6-ethoxypyridin-2-yl)methyl)-3-methyl-1H-indazol-4-amine (0.076 g, 71% yield) as a yellow gum.

후처리

  1. temperaturerefluxed for 2 hours
  2. customThe solvent was removed
  3. filtrationfiltered through glass fiber
  4. filtrationfilter paper
  5. customThe organic phase was separated
  6. customdried
  7. addition(phase separator silicone treated filter paper)
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1f317b418c6a499e865a443c815d7e6b
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09174981B2

반응 노트

불러오는 중…