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Hydroxylamine → 3-(1,3-Dioxolan-2-yl)propyl 4-(N'-hydroxycarbamimidoyl)benzoate

HRID 332709
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HRID 332709 반응식
[C:1]([C:3]1[CH:19]=[CH:18][C:6]([C:7]([O:9][CH2:10][CH2:11][CH2:12][CH:13]2[O:17][CH2:16][CH2:15][O:14]2)=[O:8])=[CH:5][CH:4]=1)#[N:2].[NH2:20][OH:21]>C(O)C.[Cl-].[Na+].O>[OH:21][N:20]=[C:1]([C:3]1[CH:4]=[CH:5][C:6]([C:7]([O:9][CH2:10][CH2:11][CH2:12][CH:13]2[O:14][CH2:15][CH2:16][O:17]2)=[O:8])=[CH:18][CH:19]=1)[NH2:2]
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참가 물질

5

반응물 2

HCID 787HydroxylamineHCID 711131693-(1,3-Dioxolan-2-yl)propyl 4-cyanobenzoate

생성물 1

HCID 866769173-(1,3-Dioxolan-2-yl)propyl 4-(N'-hydroxycarbamimidoyl)benzoate

시약·촉매·용매 2

HCID 702Ethanol용매HCID 57417360Sodium chloride; water용매

반응 조건

온도
80 °C

실험 절차

To a solution of 3-(1,3-dioxolan-2-yl)propyl 4-cyanobenzoate (1.00 g, 4.38 mmol) in ethanol (5 mL), was added hydroxylamine (50% aqueous solution, 5 mL), and the mixture heated at 80° C. for 4 hours. The reaction was diluted with saturated brine and extracted with ethyl acetate (×3). The combined organic fractions were dried with magnesium sulphate, and the solvent evaporated at reduced pressure. The material was used directly in the next step without further purification.

후처리

  1. extractionextracted with ethyl acetate (×3)
  2. dry with materialThe combined organic fractions were dried with magnesium sulphate
  3. customthe solvent evaporated at reduced pressure
  4. customThe material was used directly in the next step without further purification

출처 및 근거

ORD 기록
ord-7ac6906fe06c4bc38af0037cb23ac1c0
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08877774B2

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