Reaktion #317888

Reaktionsgleichung

3′-aminoacetophenone

methyl trifluoroacetate

water

→

3-acetyl-trifluoroacetylaminobenzene

Ausbeute 85.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeto terminate
2. 2
   Sonstigethe reaction
3. 3
   SonstigeThen, the solvent was removed under reduced pressure
4. 4
   workup.DISSOLUTIONThe residue was dissolved in 50 mL of ethyl acetate
5. 5
   Waschenwashed twice with 30 mL of water
6. 6
   Trocknendried over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONdistilled under reduced pressure

Vorschrift

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.

Quelle