Ethanol → N-[(3-phenoxyphenyl)methylidene]hydroxylamine

HRID 1659654

반응식

HRID 1659654 반응식
[O:1]([C:8]1[CH:9]=[C:10]([CH:14]2OCCO2)[CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)C.[Cl-].[OH:23][NH3+:24].O>ClC(Cl)(Cl)Cl.C1C=CC=CC=1>[O:1]([C:8]1[CH:9]=[C:10]([CH:11]=[CH:12][CH:13]=1)[CH:14]=[N:24][OH:23])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 4

HCID 702EthanolHCID 962WaterHCID 21645Hydroxylamine HClHCID 136438312-(3-Phenoxyphenyl)-1,3-dioxolane

생성물 1

HCID 2393595N-[(3-phenoxyphenyl)methylidene]hydroxylamine수율 94%

시약·촉매·용매 2

HCID 241Benzene용매HCID 5943Carbon Tetrachloride용매

실험 절차

To a solution of 24.2 g. of 2-(3-phenoxyphenyl)-1,3-dioxolane in 150 ml. of ethyl alcohol a solution of 14 g. of hydroxylammonium chloride in 150 ml. of water is added, and the mixture is boiled until no traces of starting compound can be detected by thin layer chromatography (silica gel, 1:1 mixture of benzene and tetrachloromethane, development: by UV light). Alcohol is distilled off and the aqueous residue is cooled in ice water. The precipitated crystals are filtered off. 20 g. (94%) of 3-phenoxybenzaldehyde oxime are obtained, melting at 45° to 46° C.

후처리

  1. distillationAlcohol is distilled off
  2. temperaturethe aqueous residue is cooled in ice water
  3. filtrationThe precipitated crystals are filtered off

출처 및 근거

ORD 기록
ord-35f5d7ec4b054a5cbd2d738578896b46
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04304938

연결된 노트

불러오는 중…