Hydroxyamine hydrochloride → HCID 66759309、化合物

HRID 880352ノート

反応式

HRID 880352 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:12]=[C:11]([O:23][C:24]2[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][CH:25]=2)[C:10]=1[C:33](=[O:42])[CH2:34][C:35](=O)[C:36]([O:38][CH2:39][CH3:40])=[O:37])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:44]O>C(O)C>[CH2:1]([O:8][C:9]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:12]=[C:11]([O:23][C:24]2[CH:25]=[CH:26][C:27]([N+:30]([O-:32])=[O:31])=[CH:28][CH:29]=2)[C:10]=1[C:33]1[O:42][N:44]=[C:35]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[CH:34]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 66758581Ethyl 4-[2,4-bis(benzyloxy)-6-(4-nitrophenoxy)phenyl]-2,4-dioxobutanoate

生成物 1

HCID 66759309HCID 66759309、化合物収率 82%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A stirred solution of ethyl 4-[2,4-bis(benzyloxy)-6-(4-nitrophenoxy)phenyl]-2,4-dioxobutanoate (5 g, 9 mmol) and hydroxylamine hydrochloride (0.74 g, 15 mmol, 1.2 eq) in ethanol (mL 50) was refluxed for 2 hours. The solution was concentrated to a small volume and diluted with ethyl acetate. After washing with brine and drying, the solvent was removed and the residue was carefully chromatographed on silica gel eluting with hexane/ethyl acetate 6/1, to provide the title compound (4.1 g, 82% yield).

後処理

  1. concentrationThe solution was concentrated to a small volume
  2. additiondiluted with ethyl acetate
  3. washAfter washing with brine
  4. customdrying
  5. customthe solvent was removed
  6. customthe residue was carefully chromatographed on silica gel eluting with hexane/ethyl acetate 6/1

出典と根拠

ORDレコード
ord-5c6648198cf546548555f30d815e969c
出典データセット
uspto-grants-2015_03
特許番号
US08993556B2

反応ノート

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