Ammonium Chloride → HCID 67974925、化合物

HRID 706655ノート

反応式

HRID 706655 の反応式
[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]

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 67976364HCID 67976364、化合物

生成物 1

HCID 67974925HCID 67974925、化合物収率 71.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 19096565Water ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f317b418c6a499e865a443c815d7e6b
出典データセット
uspto-grants-2015_11
特許番号
US09174981B2

反応ノート

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