Phthalic Anhydride → 3-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide

HRID 81694노트

반응식

HRID 81694 반응식
[Cl:1][C:2]1[C:3]([CH3:11])=[N:4][CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].C(N)(N)=[O:13].OO.C1(=O)OC(=O)C2=CC=CC=C12.S([O-])([O-])(=O)=S.[Na+].[Na+]>ClCCl.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([CH3:11])=[N+:4]([O-:13])[CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9]

참가 물질

7

반응물 4

HCID 6811Phthalic AnhydrideHCID 24477Sodium ThiosulfateHCID 31294Carbamide PeroxideHCID 582012143-Chloro-4-methoxy-2,5-dimethylpyridine

생성물 1

HCID 143691543-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide수율 91.5%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

The above 3-chloro-4-methoxy-2,5-dimethylpyridine (181 mg) was dissolved in 5 ml of dichloromethane, and urea peroxide (169 mg) and phthalic anhydride (219 mg) were then added to the solution. The resulting mixture was stirred at room temperature for 2.5 hours. Thereafter, a saturated aqueous sodium thiosulfate solution was added to the reaction solution under cooling on ice, and the resulting mixture was then diluted with chloroform. The water layer was extracted with chloroform two times. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (181 mg) as a solid.

후처리

  1. temperatureunder cooling on ice
  2. extractionThe water layer was extracted with chloroform two times
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. distillationthe solvent was then distilled away

출처 및 근거

ORD 기록
ord-dbb251982fd84cea88e23d9109cbe504
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846703B2

반응 노트

불러오는 중…