تفاعل #336049

معادلة التفاعل

sodium bicarbonate

4-(2,3,4,5,6-pentafluorophenoxy)piperidine

formic acid

acetic

→

1-formyl-4-(2,3,4,5,6-pentafluorophenoxy)piperidine

المردود 91.0%

المذيبات

diethyl ether

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled
2. 2
   workup.STIRRINGThe reaction mixture was then stirred at ambient temperature for three hours
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلThe organic layer was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   ترشيحFiltration
7. 7
   أخرىfollowed by evaporation of the solvent
8. 8
   أخرىafforded an oil which
9. 9
   أخرىwas purified by means of high pressure liquid chromatography (silica gel; elution with ethyl acetate)

الإجراء التجريبي

A mixture of 1.5 ml of formic acid and 3.5 ml of acetic anydride was stirred at 55° C. for one hour, cooled, and treated with a solution of 4.0 g of 4-(2,3,4,5,6-pentafluorophenoxy)piperidine in 50 ml of diethyl ether. The reaction mixture was then stirred at ambient temperature for three hours. Thereafter, the mixture was poured into 100 ml of water, adjusted to pH 10 by the addition of sodium bicarbonate, and extracted with ethyl acetate. The organic layer was washed with water followed by a saturated solution of chloride and dried over anhydrous magnesium sulfate. Filtration, followed by evaporation of the solvent afforded an oil which was purified by means of high pressure liquid chromatography (silica gel; elution with ethyl acetate) to yield 4.0 g (91%) of 1-formyl-4-(2,3,4,5,6-pentafluorophenoxy)piperidine, m.p. 32°-34° C.

المصدر