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Water → 2-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)-N'-hydroxyacetimidamide

HRID 455132
ノート
印刷プレビュー

反応式

HRID 455132 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]3[C:16]=2[CH2:17][C:18]#[N:19])=[CH:4][CH:3]=1.[NH2:20][OH:21].Cl.C([O-])([O-])=O.[K+].[K+].O>CCO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][N:11]3[C:16]=2[CH2:17][C:18](=[N:20][OH:21])[NH2:19])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 872822-(4-Chlorophenyl)imidazo(1,2-a)pyridine-3-acetonitrileHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 866551272-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)-N'-hydroxyacetimidamide

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒

実験手順

To a suspension of 2-(2-(4-chlorophenyl)imidazo[1,2-a]pyridin-3-yl)acetonitrile (0.13 mol, 34.0 g) in absolute EtOH (300 mL) was added NH2OH.HCl (0.32 mol, 22.1 g) and K2CO3 (0.32 mol, 44.1 g), respectively. The mixture was stirred at r.t. overnight, filtrated, and washed with EtOH for 3 times. The EtOH-filtrate was concertrated to small volume, and the precipitation was collected by filtration, to give one partial products. The solid was dispersed into water, sonicated for 10 mins, filtrated, washed with water, and dried in vacuo, to give another partial products. Combined two portions products added up to 25.0 g (65.4%). m/e+=301 (M+H+).

後処理

  1. filtrationfiltrated
  2. washwashed with EtOH for 3 times
  3. customthe precipitation
  4. filtrationwas collected by filtration
  5. customto give one partial products
  6. customsonicated for 10 mins
  7. filtrationfiltrated
  8. washwashed with water
  9. customdried in vacuo
  10. customto give another partial products
  11. additionadded up to 25.0 g (65.4%)

出典と根拠

ORDレコード
ord-203af166414a43e1b731287c43365ba9
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08497278B2

反応ノート

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