Sodium Hydroxide → N-Hydroxybenzo[d][1,3]dioxole-5-carboximidamide

HRID 538607

反応式

HRID 538607 の反応式
O1[C:5]2[CH:6]=[CH:7][C:8]([C:10]#[N:11])=[CH:9][C:4]=2[O:3][CH2:2]1.Cl.[NH2:13][OH:14].[OH-:15].[Na+]>CCO>[OH:14][NH:13][C:10]([C:8]1[CH:7]=[CH:6][C:5]2[O:15][CH2:2][O:3][C:4]=2[CH:9]=1)=[NH:11]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 78136Benzo-1,3-dioxole-5-carbonitrileHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 178513224N-Hydroxybenzo[d][1,3]dioxole-5-carboximidamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of Benzo[1,3]dioxole-5-carbonitrile (5.0 g, 33.9 mmol) in EtOH (100 mL) was added hydroxylamine hydrochloride (4.68 g, 67.90 mmol) and NaOH (2.71 g, 67.9 mmol). The resulting reaction mixture was refluxed for 12 h. After the completion of the reaction (TLC monitoring), the mixture was concentrated, added EtOH and filtered. The filtrate was evaporated under reduced pressure and used as such for the next step (crude yield 4.8 g, 78.68%).

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas refluxed for 12 h
  3. customAfter the completion of the reaction (TLC monitoring)
  4. concentrationthe mixture was concentrated
  5. additionadded EtOH
  6. filtrationfiltered
  7. customThe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-ed4964eb1abe4136a714c129c4b0a833
出典データセット
uspto-grants-2014_10
特許番号
US08865736B2

関連ノート

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