反应 #554636

反应方程式

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

sodium acetate

→

compound

收率 78.5%

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

收率 78.5%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   温度The reaction solution was cooled down to room temperature
2. 2
   萃取extracted with ethyl acetate (600 ml×6)
3. 3
   洗涤washed three times with brine
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   浓缩concentrated
6. 6
   其他until dry
7. 7
   其他The residue was crystallized from the mixed toluene/petroleum ether solution
8. 8
   其他dried

实验过程

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].

来源