Water → Acetanilide, 3'-acetyl-2,2,2-trifluoro-

HRID 230706

Reaktionsgleichung

Reaktionsgleichung von HRID 230706
[NH2:1][C:2]1[CH:3]=[C:4]([C:8](=[O:10])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[F:11][C:12]([F:18])([F:17])[C:13](OC)=[O:14].O>CO>[C:8]([C:4]1[CH:3]=[C:2]([NH:1][C:13](=[O:14])[C:12]([F:18])([F:17])[F:11])[CH:7]=[CH:6][CH:5]=1)(=[O:10])[CH3:9]

Komponenten

5

Edukt 3

HCID 962WaterHCID 74173'-AminoacetophenoneHCID 9893Methyl trifluoroacetate

Produkt 1

HCID 673706Acetanilide, 3'-acetyl-2,2,2-trifluoro-Ausbeute 85 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

10 mmol of 3′-aminoacetophenone as a starting material was dissolved in a methanol solvent in a 100 mL round-bottomed flask and 1.2 equivalents (eq) of methyl trifluoroacetate was added dropwise thereto over 30 minutes at room temperature, and subsequently the reaction mixture was stirred for 2 hours. After the completion of the reaction was confirmed by TLC, a small amount of water was added to terminate the reaction. Then, the solvent was removed under reduced pressure. The residue was dissolved in 50 mL of ethyl acetate and washed twice with 30 mL of water, dried over anhydrous sodium sulfate, and distilled under reduced pressure to obtain the desired 3-acetyl-trifluoroacetylaminobenzene (85%) as a brown oil.

Aufarbeitung

  1. customto terminate
  2. customthe reaction
  3. customThen, the solvent was removed under reduced pressure
  4. dissolutionThe residue was dissolved in 50 mL of ethyl acetate
  5. washwashed twice with 30 mL of water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-765ccfd9ba554e248b48d58848b357ce
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07566773B2

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