تفاعل #84284

معادلة التفاعل

water

2-bromo-1-(3-chloro-5-methoxypyridin-2-yl)ethanone

potassium phthalimide

potassium iodide

→

desired product

المردود 16.8%

N-[2-(3-chloro-5-methoxypyridin-2-yl)-2-oxoethyl]phthalimide

المردود 16.8%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter completion of the reaction
2. 2
   درجة الحرارةto cool to room temperature
3. 3
   استخلاصextracted with ethyl acetate (40 ml×1)
4. 4
   تجفيفthe resulting organic layer was dried over saturated aqueous sodium chloride
5. 5
   أخرىanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
6. 6
   أخرىThe resulting residue was purified by silica gel column chromatography

الإجراء التجريبي

To 570 mg of 2-bromo-1-(3-chloro-5-methoxypyridin-2-yl)ethanone in 10 ml of N,N-dimethylformamide, 800 mg of potassium phthalimide and 36 mg of potassium iodide were added, and the mixture was stirred at 80° C. for 5 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 20 ml of water and extracted with ethyl acetate (40 ml×1), the resulting organic layer was dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 0.12 g of the desired product as white crystals.

المصدر