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

HRID 1609263ノート

反応式

HRID 1609263 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-813a322781a5422fa36680d115afb337
出典データセット
uspto-grants-1995_03
特許番号
US05399703

反応ノート

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