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

HRID 538607

반응식

HRID 538607 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ed4964eb1abe4136a714c129c4b0a833
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865736B2

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