Reaktion #554636

Reaktionsgleichung

2-chloro-1-(4-fluorophenyl)ethanone

sodium acetate

→

compound

Ausbeute 78.5%

[2-(4-fluorophenyl)-2-oxo-ethyl]acetate

Ausbeute 78.5%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction solution was cooled down to room temperature
2. 2
   Extraktionextracted with ethyl acetate (600 ml×6)
3. 3
   Waschenwashed three times with brine
4. 4
   Trocknendried over anhydrous sodium sulfate
5. 5
   Einengenconcentrated
6. 6
   Sonstigeuntil dry
7. 7
   SonstigeThe residue was crystallized from the mixed toluene/petroleum ether solution
8. 8
   Sonstigedried

Vorschrift

To a 3 liter flask were added 400 grams (2.32 mol) 2-chloro-1-(4-fluorophenyl)ethanone, 1 liter of N,N-dimethylformamide and 265 grams (3.23 mol) anhydrous sodium acetate. The mixture was stirred and heated to 90° C., and the reaction lasted 10 hours. After the reaction was completed, the heating was stopped. The reaction solution was cooled down to room temperature, and extracted with ethyl acetate (600 ml×6). The organic phases were combined, washed three times with brine, dried over anhydrous sodium sulfate and concentrated until dry. The residue was crystallized from the mixed toluene/petroleum ether solution and dried to obtain 357 grams (1.82 mol) compound A-1 with yield of 78.5%. 1H NMR (400 MHz, CDCl3): δ 2.23 (s, 3H, CH3), 5.30 (s, 2H, —CH2—), 7.14-7.19 (m, 2H, Cpr-H), 7.93-7.97 (m, 2H, Cpr-H); MS (m/z): 197 [M+H].

Quelle