Trifluoroacetic anhydride → HCID 58201206, 화합물

HRID 2408896노트

반응식

HRID 2408896 반응식
[Cl:1][C:2]1[C:3]([CH3:12])=[N+:4]([O-])[CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].FC(F)(F)C(OC(=O)C(F)(F)F)=[O:16]>ClCCl.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:3]([CH2:12][OH:16])=[N:4][CH:5]=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9]

참가 물질

5

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 143691543-Chloro-4-methoxy-2,5-dimethylpyridine 1-oxide

생성물 1

HCID 58201206HCID 58201206, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

The above 3-chloro-4-methoxy-2,5-dimethylpyridine 1-oxide (530 mg) was suspended in 15 ml of dichloromethane, and trifluoroacetic anhydride (0.39 ml) was then added to the suspension under cooling on ice. The resulting mixture was stirred at room temperature for 3 hours. The reaction solution was diluted with chloroform, and was then washed with a saturated sodium bicarbonate solution. The water layer was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was then distilled away, so as to obtain the title compound (521 mg) as an oily substance.

후처리

  1. temperatureunder cooling on ice
  2. washwas then washed with a saturated sodium bicarbonate solution
  3. extractionThe water layer was extracted with chloroform
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. distillationthe solvent was then distilled away

출처 및 근거

ORD 기록
ord-cf553cae97b24d06b4c063f02faf80b7
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08815880B2

반응 노트

불러오는 중…