Trifluoroacetic anhydride → 2-[3-(2-Nitrophenoxy)phenoxy]propionitrile

HRID 1609263노트

반응식

HRID 1609263 반응식
[N+:1]([C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:16]=[CH:17][CH:18]=1)[O:10][CH:11]([CH3:15])[C:12]([NH2:14])=O)([O-:3])=[O:2].FC(F)(F)C(OC(=O)C(F)(F)F)=O>N1C=CC=CC=1.O1CCOCC1>[N+:1]([C:4]1[CH:22]=[CH:21][CH:20]=[CH:19][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:16]=[CH:17][CH:18]=1)[O:10][CH:11]([CH3:15])[C:12]#[N:14])([O-:3])=[O:2]

참가 물질

5

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 200843872-[3-(2-Nitrophenoxy)phenoxy]propionamide

생성물 1

HCID 200844962-[3-(2-Nitrophenoxy)phenoxy]propionitrile수율 100.5%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 312751,4-Dioxane용매

실험 절차

In a mixture of 12 ml of pyridine and 35 ml of dioxane was suspended 4.55 g of 2-[3-(2-nitrophenoxy)phenoxy]propionamide and, then, 3.6 g of trifluoroacetic anhydride was added dropwise with ice-cooling and stirring. The mixture was then stirred at that temperature for 30 minutes and, following addition of ice-water, extracted with ether. The ether extract was washed with diluted hydrochloric acid and sodium hydrogen carbonate solution in that order, dried and concentrated to give 4.3 g of the title compound as a light yellow oil.

후처리

  1. temperaturecooling
  2. stirringThe mixture was then stirred at that temperature for 30 minutes
  3. extractionextracted with ether
  4. extractionThe ether extract
  5. washwas washed with diluted hydrochloric acid and sodium hydrogen carbonate solution in that order
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-813a322781a5422fa36680d115afb337
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05399703

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