반응 #2304287

반응 방정식

3-[(6-bromohexyloxy)methyl]-3-methyloxetane

ethyl 4-hydroxybenzoate

potassium carbonate

dimethylformamide

→

ethyl 4-[6-(3-methyloxetan-3-ylmethoxy)hexyloxy]benzoate

수율 80.6%

용매

Water

반응 조건

후처리

1. 1
   추출This was extracted with ethyl acetate
2. 2
   세척the organic layer was washed with aqueous 2 N-sodium hydroxide solution and water in that order
3. 3
   건조dried with anhydrous magnesium sulfate
4. 4
   기타The solvent was evaporated away
5. 5
   기타the resulting residue was purified through silica gel chromatography (elution solvent:toluene/ethyl acetate=8/2)

실험 절차

A reaction mixture comprising 84 g of 3-[(6-bromohexyloxy)methyl]-3-methyloxetane, 50 g of ethyl 4-hydroxybenzoate, 50 g of potassium carbonate and 600 ml of dimethylformamide was stirred at 90° C. for 4 hours. Water was added to the reaction mixture and the reaction was stopped. This was extracted with ethyl acetate, and the organic layer was washed with aqueous 2 N-sodium hydroxide solution and water in that order, and then dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was purified through silica gel chromatography (elution solvent:toluene/ethyl acetate=8/2), and 85 g of ethyl 4-[6-(3-methyloxetan-3-ylmethoxy)hexyloxy]benzoate was obtained.

출처