Sodium Hydroxide → 3,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

HRID 1497027노트

반응식

HRID 1497027 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])[C:5]#[N:6].Cl.[NH2:12][OH:13].[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[Cl:10])/[C:5](=[N:12]/[OH:13])/[NH2:6]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 810513,4-DichlorobenzonitrileHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 112641853,4-Dichloro-N'-hydroxybenzene-1-carboximidamide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 3,4-dichlorobenzonitrile (2.00 g, 11.6 mmol), hydroxylamine hydrochloride (1.65 mL, 12.8 mmol) and sodium hydroxide (4.15 mL, 12.4 mmol) in ethanol (40 mL) was stirred at rt for 1 h. The reaction mixture was concentrated and refluxed in hexanes for 30 min and concentrated in vacuo. The product, intermediate 33A was used directly without purification. HPLC/MS (Method C) retention time=1.24 min [M+H]+204.9.

후처리

  1. concentrationThe reaction mixture was concentrated
  2. temperaturerefluxed in hexanes for 30 min
  3. concentrationconcentrated in vacuo
  4. customThe product, intermediate 33A was used directly without purification

출처 및 근거

ORD 기록
ord-f4a465105da645639c3b9a45d21426d2
출처 데이터셋
uspto-grants-2015_12
특허 번호
US09199946B2

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