Hydroxyamine hydrochloride → HCID 85613806, 화합물

HRID 466186

반응식

HRID 466186 반응식
[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]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 14971313HCID 14971313, 화합물

생성물 1

HCID 85613806HCID 85613806, 화합물

시약·촉매·용매 1

HCID 21975839Pyridine ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-0152ccd687c04e58ac7554e776404ca2
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155130

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