反応 #1674869

反応方程式

hexyl 3-hexyloxypicolinate

potassium hydroxide

→

oily product

収率 111.1%

3-hexyloxypicolinic acid

収率 111.1%

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度by refluxing for 1.5 hours
3. 3
   workup.DISTILLATIONThe solvent was distilled off under a reduced pressure
4. 4
   workup.DISSOLUTIONthe residue was dissolved in 30 ml of water
5. 5
   抽出was extracted with dichloromethane
6. 6
   乾燥After drying over anhydrous sodium sulfate
7. 7
   workup.DISTILLATIONthe solvent was distilled off

実験手順

In 10 ml of methanol was dissolved 2.50 g (8.1 mmol) of hexyl 3-hexyloxypicolinate and 10 ml of a 10% potassium hydroxide solution was added thereto, followed by refluxing for 1.5 hours. The solvent was distilled off under a reduced pressure and the residue was dissolved in 30 ml of water and, after the pH of the solution was adjusted to about 2 with 6N hydrochloric acid, was extracted with dichloromethane. After drying over anhydrous sodium sulfate, the solvent was distilled off to obtain 2.01 g of an oily product. Since the recrystallization cannot be effected in any solvents, the washing with hexane was repeated to obtain 0.80 g of the oily product, which was directly used in the subsequent reaction.

出典