Benzyloxyamine hydrochloride → HCID 86606488, 화합물

HRID 2055204노트

반응식

HRID 2055204 반응식
[CH3:1][O:2][C:3]([C:5]1([CH:13]=O)[CH2:8][CH:7]([CH2:9][CH2:10][CH2:11][CH3:12])[CH2:6]1)=[O:4].C([O-])(=O)C.[Na+].Cl.[CH2:21]([O:28][NH2:29])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CO>[CH3:1][O:2][C:3]([C:5]1([CH:13]=[N:29][O:28][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:6][CH:7]([CH2:9][CH2:10][CH2:11][CH3:12])[CH2:8]1)=[O:4]

참가 물질

5

반응물 3

HCID 102312Benzyloxyamine hydrochlorideHCID 517045Sodium AcetateHCID 71416977Methyl 3-butyl-1-formylcyclobutane-1-carboxylate

생성물 1

HCID 86606488HCID 86606488, 화합물수율 64.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 3-butyl-1-formyl-cyclobutanecarboxylic acid methyl ester (7.2 g, 36.7 mmol), sodium acetate (6.1 g, 73.4 mmol) and O-benzylhydroxylamine hydrochloride (11.9 g, 73.4 mmol) were stirred in methanol (90 mL) for 18 h. The methanol was removed in vacuo, water (100 mL) was added and the aqueous phase was extracted with EtOAc (75 mL×5). The combined organic extracts were dried (MgSO4) and were evaporated in vacuo. The residue was purified by flash column chromatography using an eluting system of hexane/EtOAc (9:1) to yield the title compound as a clear colorless oil (7.23 g, 64%). MH+304.

후처리

  1. customThe methanol was removed in vacuo, water (100 mL)
  2. additionwas added
  3. extractionthe aqueous phase was extracted with EtOAc (75 mL×5)
  4. dry with materialThe combined organic extracts were dried (MgSO4)
  5. customwere evaporated in vacuo
  6. customThe residue was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-b771c875c3064ffaaee46eefe68c156e
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07332485B2

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