반응 #2069931

반응 방정식

dimethylformamide

allyl (4-chlorobutyl) ether

4-hydroxybenzoic acid

potassium carbonate

→

4-(4-allyloxybutyloxy)benzoic acid

수율 123.0%

용매

Water

반응 조건

후처리

1. 1
   추출extracted with toluene
2. 2
   세척the toluene layer was well washed with water, and toluene
3. 3
   기타was 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
   온도refluxed for 2 hours
6. 6
   기타Ethanol was evaporated away
7. 7
   workup.ADDITIONhydrochloric acid was added
8. 8
   추출extracted with diethyl ether
9. 9
   건조dried with anhydrous magnesium sulfate
10. 10
    기타The solvent was evaporated away
11. 11
    기타the resulting residue was recrystallized from a mixed solvent of ethanol and water

실험 절차

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.

출처