反応 #336049

反応方程式

sodium bicarbonate

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

formic acid

acetic

→

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

収率 91.0%

溶媒

diethyl ether

water

反応条件

後処理

1. 1
   温度cooled
2. 2
   workup.STIRRINGThe reaction mixture was then stirred at ambient temperature for three hours
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The organic layer was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   ろ過Filtration
7. 7
   その他followed by evaporation of the solvent
8. 8
   その他afforded an oil which
9. 9
   その他was purified by means of high pressure liquid chromatography (silica gel; elution with ethyl acetate)

実験手順

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.

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