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Hydroxyamine hydrochloride → 1-(5-Benzyl-5-azaspiro[2.4]hept-7-yl)ethanone oxime

HRID 10345
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반응식

HRID 10345 반응식
[CH2:1]([N:8]1[CH2:14][CH:13]([C:15](=O)[CH3:16])[C:10]2([CH2:12][CH2:11]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:19][OH:20]>N1C=CC=CC=1.C(OCC)(=O)C>[CH2:1]([N:8]1[CH2:14][CH:13]([C:15](=[N:19][OH:20])[CH3:16])[C:10]2([CH2:12][CH2:11]2)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 21978858HCID 21978858, 화합물

생성물 1

HCID 723905271-(5-Benzyl-5-azaspiro[2.4]hept-7-yl)ethanone oxime수율 73.5%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

1-(5-benzyl-5-azaspiro[2.4]hept-7-yl)ethanone (Example A2a, 3.93 g, 17.1 mmol) and hydroxylamine hydrochloride (1.78 g, 25.7 mmol) are stirred in pyridine (10 mL) at 90° C. After 20 hours, the reaction mixture is diluted with ethyl acetate and the organic layer is washed with saturated NaHCO3, water, and brine. The organic layer is dried with MgSO4, filtered, and the filtrate concentrated to afford 1-(5-benzyl-5-azaspiro[2.4]hept-7-yl)ethanone oxime as an oil (3.07 g). MSCI: m/z 245 (MH+).

후처리

  1. washthe organic layer is washed with saturated NaHCO3, water, and brine
  2. dry with materialThe organic layer is dried with MgSO4
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated

출처 및 근거

ORD 기록
ord-eebca15bfe1a40339125a48548988faa
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07094780B1

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