반응 #742250

반응 방정식

3-[5-methyl-2-(tetrahydro-pyran-2-yloxy)-phenyl]-acrylic acid ethyl ester

p-toluenesulfonic acid

→

colourless crystals

수율 71.0%

(E)-3-(2-Hydroxy-5-methyl-phenyl)-acrylic acid ethyl ester

수율 71.0%

용매

ethanol

반응 조건

후처리

1. 1
   농축Then the reaction mixture was concentrated
2. 2
   workup.ADDITIONthe residue was diluted with ether
3. 3
   세척washed with saturated sodium bicarbonate and brine
4. 4
   기타dried
5. 5
   기타evaporated to dryness
6. 6
   기타The resulting yellow solid was recrystallized

실험 절차

A solution of 193.7 g 3-[5-methyl-2-(tetrahydro-pyran-2-yloxy)-phenyl]-acrylic acid ethyl ester (Bunce, R., Moore, J., Org. Prep. Proc., 29(3), 293 (1997)) and 2 g p-toluenesulfonic acid in 2.5 l of ethanol was stirred at room temperature for 24 hours. Then the reaction mixture was concentrated and the residue was diluted with ether, washed with saturated sodium bicarbonate and brine, dried and evaporated to dryness. The resulting yellow solid was recrystallized to yield 97.7 g of colourless crystals.

출처