反応 #2069931

反応方程式

dimethylformamide

allyl (4-chlorobutyl) ether

4-hydroxybenzoic acid

potassium carbonate

→

4-(4-allyloxybutyloxy)benzoic acid

収率 123.0%

溶媒

Water

反応条件

後処理

1. 1
   抽出extracted with toluene
2. 2
   洗浄the toluene layer was well washed with water, and toluene
3. 3
   その他was evaporated away
4. 4
   workup.ADDITION20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue
5. 5
   温度refluxed for 2 hours
6. 6
   その他Ethanol was evaporated away
7. 7
   workup.ADDITIONhydrochloric acid was added
8. 8
   抽出extracted with diethyl ether
9. 9
   乾燥dried with anhydrous magnesium sulfate
10. 10
    その他The solvent was evaporated away
11. 11
    その他the resulting residue was recrystallized from a mixed solvent of ethanol and water

実験手順

A solution comprising 14 g of allyl (4-chlorobutyl) ether, 14 g of 4-hydroxybenzoic acid, 14 g of potassium carbonate and 50 ml of dimethylformamide was stirred at 90° C. for 3 hours. Water was added to it, and extracted with toluene, and the toluene layer was well washed with water, and toluene was evaporated away. 20 g of sodium hydroxide, 50 ml of water and 200 ml of ethanol were added to the resulting residue, and refluxed for 2 hours. Ethanol was evaporated away, and hydrochloric acid was added to make it acidic, and then extracted with diethyl ether and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was recrystallized from a mixed solvent of ethanol and water to obtain 29 g of 4-(4-allyloxybutyloxy)benzoic acid.

出典