تفاعل #11748

معادلة التفاعل

2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone

(5-chloro-2-hydroxy-phenyl)-acetic acid ethyl ester

potassium carbonate

potassium iodide

→

title compound

المردود 97.8%

(5-Chloro-2-{2-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-phenyl)-acetic acid ethyl ester

المردود 97.8%

المذيبات

ethyl acetate

2-butanone

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction was heated
2. 2
   درجة الحرارةat reflux for 48 hrs
3. 3
   درجة الحرارةThe solution was cooled
4. 4
   غسيلwashed with brine
5. 5
   تجفيفThe organic layer was dried over magnesium sulfate
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated in vacuo
8. 8
   أخرىThe crude product was purified
9. 9
   workup.DISSOLUTIONby dissolving in dichloromethane
10. 10
    تركيزConcentration in vacuo

الإجراء التجريبي

To a solution of 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (3.3 g, 11.0 mmol) in 2-butanone (100 mL) was added (5-chloro-2-hydroxy-phenyl)-acetic acid ethyl ester (2.3 g, 11.0 mmol), potassium carbonate (3.05 g, 22.1 mmol), and potassium iodide (1.83 g, 11.0 mmol). The reaction was heated at reflux for 48 hrs. The solution was cooled, diluted with ethyl acetate and washed with brine. The organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The crude product was purified by dissolving in dichloromethane and passing through a pad of silica gel. Concentration in vacuo gave the title compound (5.13 g).

المصدر