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

HRID 415681

반응식

HRID 415681 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-9b061b4b990849b49c3f77d2212db2d9
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088791B2

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