Hydroxylamine → 4-((1,3-Dioxolan-2-yl)methyl)-N'-hydroxybenzimidamide

HRID 332696노트

반응식

HRID 332696 반응식
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][CH:8]=1.[NH2:15][OH:16]>C(O)C>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[CH2:6][C:7]1[CH:14]=[CH:13][C:10]([C:11](=[N:15][OH:16])[NH2:12])=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 38007934-((1,3-Dioxolan-2-yl)methyl)benzonitrile

생성물 1

HCID 866769114-((1,3-Dioxolan-2-yl)methyl)-N'-hydroxybenzimidamide수율 73%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4-((1,3-dioxolan-2-yl)methyl)benzonitrile (1.40 g, 7.41 mmol) in ethanol (10 mL), was added 50% aqueous hydroxylamine (5 mL), and the resultant mixture was heated at 80° C. for 16 hours. The solvent was evaporated at reduced pressure, and the residue partitioned between ethyl acetate and brine. The organic phase was removed, and the aqueous phase was extracted with further ethyl acetate (×2). The combined organic extracts were dried with aqueous magnesium sulfate and evaporated at reduced pressure to afford the title compound (1.21 g, 73%).

후처리

  1. customThe solvent was evaporated at reduced pressure
  2. customthe residue partitioned between ethyl acetate and brine
  3. customThe organic phase was removed
  4. extractionthe aqueous phase was extracted with further ethyl acetate (×2)
  5. dry with materialThe combined organic extracts were dried with aqueous magnesium sulfate
  6. customevaporated at reduced pressure

출처 및 근거

ORD 기록
ord-9414414e55cd49c29ed4f6c7d8985207
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877774B2

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