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

HRID 568718노트

반응식

HRID 568718 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 LC 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 LC System 500 using 5% ethyl acetate/toluene as the eluting system

출처 및 근거

ORD 기록
ord-784590844a3b48899b8f29094a83080e
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728662

반응 노트

불러오는 중…