تفاعل #84279

معادلة التفاعل

water

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

ethoxyamine hydrochloride

→

desired product

المردود 46.4%

N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-(ethoxyimino)ethyl]phthalimide

المردود 46.4%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter completion of the reaction
2. 2
   استخلاصextracted with ethyl acetate (5 ml×3)
3. 3
   تجفيفdried over saturated aqueous sodium chloride
4. 4
   أخرىanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
5. 5
   أخرىThe resulting residue was purified by preparative medium pressure liquid chromatography (preparative medium pressure chromatograph: YFLC-Wprep manufactured by Yamazen Science, Inc.)

الإجراء التجريبي

To 214 mg of the N-[2-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]-2-oxoethyl]phthalimide prepared in Step 2 in Synthetic Example 6 in 3 ml of ethanol, 84 mg of ethoxyamine hydrochloride was added, and the mixture was stirred at room temperature for 18 hours. After completion of the reaction, the reaction mixture was mixed with 5 ml of water and extracted with ethyl acetate (5 ml×3), and the resulting organic layers were combined, 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 preparative medium pressure liquid chromatography (preparative medium pressure chromatograph: YFLC-Wprep manufactured by Yamazen Science, Inc.) using ethyl acetate-hexane (with a gradient of from 2:18 to 5:15) as the eluent to obtain 111 mg of the desired product as a brown resinous substance.

المصدر