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Benzonitrile, m-chloro- → 3-Chlorobenzamidoxime

HRID 732105
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인쇄 미리보기

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HRID 732105 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[C:5]#[N:6].Cl.[NH2:11][OH:12].[OH-].[Na+]>C(O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:5](=[N:11][OH:12])[NH2:6])[CH:7]=[CH:8][CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 13015Benzonitrile, m-chloro-HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 27948173-Chlorobenzamidoxime수율 93%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

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온도
90 °C

실험 절차

A solution of 3.35 mL (30.0 mmol) 3-chlorobenzonitrile in ethanol (40 mL) was added to a solution of 2.47 g (35.5 mmol) hydroxylamine hydrochloride and 1.42 g (35.5 mmol) NaOH in water (20 mL) at r.t. and then heated at 90° C. for 24 h. After cooling, the reaction mixture was concentrated, the residue diluted with water, followed by filtration and drying to afford 1.13 g (93%) of the title compound. 1H NMR: 8.11 (s, 1H), 7.72 (s, 1H), 7.61 (m, 1H), 7.46 (m, 1H), 7.36 (m, 1H).

후처리

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture was concentrated
  3. additionthe residue diluted with water
  4. filtrationfollowed by filtration
  5. customdrying

출처 및 근거

ORD 기록
ord-984eed0d5b914057b9a2f2df9a258a65
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07585881B2

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