4'-Chloro-2-hydroxy-4-methoxybenzophenone → 2-[(E)-C-(4-chlorophenyl)-N-hydroxycarbonimidoyl]-5-methoxyphenol

HRID 652949노트

반응식

HRID 652949 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1.Cl.[NH2:20][OH:21]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5](/[C:8](=[N:20]\[OH:21])/[C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][C:10]=2[OH:17])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 665574'-Chloro-2-hydroxy-4-methoxybenzophenoneHCID 443297Hydroxyamine hydrochloride

생성물 1

HCID 1364774242-[(E)-C-(4-chlorophenyl)-N-hydroxycarbonimidoyl]-5-methoxyphenol

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 382 g of 4'-chloro-2-hydroxy-4-methoxybenzophenone, 230 g hydroxylamine hydrochloride and 1.5 liters of pyridine is heated under reflux for 3 hr. The solvent is evaporated and the residue is partitioned between hydrochloric acid and ethyl acetate. The organic extracts are combined and washed with saturated sodium chloride solution. The solvent is removed to afford a mixture of E- and Z-oxime isomers which is separated on a Waters Prep IC System 500 using 5% ethyl acetate/toluene as the eluting system to afford E-4'-chloro-2-hydroxy-4-methoxybenzophenone oxime, mp 159° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 3 hr
  3. customThe solvent is evaporated
  4. customthe residue is partitioned between hydrochloric acid and ethyl acetate
  5. washwashed with saturated sodium chloride solution
  6. customThe solvent is removed
  7. customto afford
  8. customis separated on a Waters Prep IC System 500 using 5% ethyl acetate/toluene as the eluting system

출처 및 근거

ORD 기록
ord-7f4e40c9dec042a39ba93725c6bc7fca
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673746

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