Hydroxyamine hydrochloride → HCID 85613806、化合物

HRID 466186

反応式

HRID 466186 の反応式
[C:1]([C:4]1[CH2:5][O:6][C:7]2[CH:13]=[CH:12][C:11]([O:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:10][C:8]=2[CH:9]=1)(=O)[CH3:2].Cl.[NH2:22][OH:23]>CCO.N1C=CC=CC=1>[C:1](=[N:22][OH:23])([C:4]1[CH2:5][O:6][C:7]2[CH:13]=[CH:12][C:11]([O:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:10][C:8]=2[CH:9]=1)[CH3:2]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 14971313HCID 14971313、化合物

生成物 1

HCID 85613806HCID 85613806、化合物

試薬・触媒・溶媒 1

HCID 21975839Pyridine ethanol溶媒

実験手順

The ketone (2.53 g, 9.5 mmol) is dissolved in 90 ml of an EtOH/pyridine mixture (1:1), and treated with hydroxylamine hydrochloride (0.99 g, 14.3 mmol). The mixture is stirred for 2 days. The reaction mixture is partitioned between ether and water, and the aqueous layer is extracted twice with ether. The combined organic layer is then washed twice with 2N HCl and water, dried (MgSO4), and evaporated. The residue is purified by flash chromatography (10% EtOAc/hexane) to give 3-acetyl-6-phenoxy-2H-1-benzopyran oxime as a crystalline solid.

後処理

  1. customThe reaction mixture is partitioned between ether and water
  2. extractionthe aqueous layer is extracted twice with ether
  3. washThe combined organic layer is then washed twice with 2N HCl and water
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe residue is purified by flash chromatography (10% EtOAc/hexane)

出典と根拠

ORDレコード
ord-0152ccd687c04e58ac7554e776404ca2
出典データセット
uspto-grants-1992_10
特許番号
US05155130

関連ノート

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