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

HRID 332696ノート

反応式

HRID 332696 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9414414e55cd49c29ed4f6c7d8985207
出典データセット
uspto-grants-2014_11
特許番号
US08877774B2

反応ノート

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