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Hydroxyamine hydrochloride → Benzyl N-allyl-N-[2-hydroxyiminoethyl]carbamate

HRID 876719
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인쇄 미리보기

반응식

HRID 876719 반응식
[CH2:1]([N:4]([CH2:15][CH:16]=O)[C:5](=[O:14])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH:2]=[CH2:3].Cl.[NH2:19][OH:20].O.O.O.C([O-])(=O)C.[Na+]>C(#N)C.O>[CH2:1]([N:4]([CH2:15][CH:16]=[N:19][OH:20])[C:5](=[O:14])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 23665404Sodium Acetate TrihydrateHCID 57415664Benzyl allyl(2-oxoethyl)carbamate

생성물 1

HCID 74074414Benzyl N-allyl-N-[2-hydroxyiminoethyl]carbamate수율 90.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6342
Acetonitrile
용매

실험 절차

A solution of benzyl N-allyl-N-(2-oxoethyl)carbamate (25 g, 107 mmol) in acetonitrile (150 mL) is treated with hydroxylamine hydrochloride (9.68 g, 139 mmol) and a solution of sodium acetate trihydrate (16 g, 117.9 mmol) in water (75 mL). The mixture is stirred at room temperature overnight. The acetonitrile is evaporated and the aqueous solution is extracted with ethyl acetate. The organic layer is separated, dried over magnesium sulfate, and concentrated under vacuum to give the title compound (24 g, 90%). ES/MS (m/e): 249 (M+H).

후처리

  1. customThe acetonitrile is evaporated
  2. extractionthe aqueous solution is extracted with ethyl acetate
  3. customThe organic layer is separated
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-e7b0a387b6ed4cdbbb59f36fc4f8aeee
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987254B2

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