Acetic Anhydride → [(E)-[(3-chloro-2-hydroxy-4-methoxyphenyl)-(2-fluorophenyl)methylidene]amino] acetate

HRID 568668노트

반응식

HRID 568668 반응식
[Cl:1][C:2]1[C:3]([OH:20])=[C:4]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])/[C:5](=[N:13]\[OH:14])/[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12].[C:21](OC(=O)C)(=[O:23])[CH3:22].C([O-])(O)=O.[Na+]>CCOCC>[C:21]([O:14]/[N:13]=[C:5](/[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])\[C:4]1[CH:15]=[CH:16][C:17]([O:18][CH3:19])=[C:2]([Cl:1])[C:3]=1[OH:20])(=[O:23])[CH3:22]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 1364774092-chloro-6-[(E)-C-(2-fluorophenyl)-N-hydroxycarbonimidoyl]-3-methoxyphenol

생성물 1

HCID 136477412[(E)-[(3-chloro-2-hydroxy-4-methoxyphenyl)-(2-fluorophenyl)methylidene]amino] acetate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

E-3-chloro-2'-fluoro-2-hydroxy-4-methoxybenzophenone oxime (18.1 g) is warmed at 60° C. for 30 minutes with 9 ml of acetic anhydride. The reaction mixture is distributed between ether and 10% NaHCO3 and washed with 10% NaHCO3 until the washes remained basic. Drying, evaporation and trituration with hexane gives E-3-chloro-2'-fluoro-2-hydroxy-4-methoxybenzophenone O-acetyl oxime, mp 125°-128° C.

후처리

  1. washwashed with 10% NaHCO3 until the washes
  2. customDrying
  3. customevaporation and trituration with hexane

출처 및 근거

ORD 기록
ord-3d47532432f24e5bb30b06e67acd657e
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04728662

반응 노트

불러오는 중…