تفاعل #84255

معادلة التفاعل

2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone

ethoxyamine hydrochloride

→

desired product

المردود 87.1%

2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone-O-ethyloxime

المردود 87.1%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter completion of the reaction
2. 2
   أخرىthe solvent was evaporated under reduced pressure
3. 3
   workup.ADDITIONthe resulting residue was mixed with 50 ml of water
4. 4
   استخلاصextracted with ethyl acetate (50 ml×2)
5. 5
   غسيلwashed with water (50 ml×1)
6. 6
   تجفيفdried over saturated aqueous sodium chloride
7. 7
   أخرىanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
8. 8
   أخرىThe resulting residue was purified by silica gel column chromatograph

الإجراء التجريبي

To 3.00 g of 2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone in 25 ml of ethanol, 1.09 g of ethoxyamine hydrochloride was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the solvent was evaporated under reduced pressure, the resulting residue was mixed with 50 ml of water and extracted with ethyl acetate (50 ml×2), the resulting organic layers were combined, washed with water (50 ml×1) and 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 chromatograph using ethyl acetate-hexane (with a gradient of from 5:95 to 15:85) as the eluent to obtain 3.03 g of the desired product as a colorless oil.

المصدر