Hydroxyamine hydrochloride → HCID 66759309, 화합물

HRID 880352노트

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HRID 880352 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 66759309HCID 66759309, 화합물수율 82%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5c6648198cf546548555f30d815e969c
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993556B2

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