반응 #80608

반응 방정식

2-(3-chloro-4-methoxyphenyl)-4-hydroxy-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-4,5-dihydro-1H-imidazole

p-toluenesulfonic acid monohydrate

→

2-(3-chloro-4-methoxyphenyl)-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-1H-imidazole

용매

toluene

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도to reflux for 72 hours
3. 3
   온도The reaction mixture is cooled
4. 4
   기타the solvent removed under reduced pressure
5. 5
   workup.DISSOLUTIONThe crude residue is redissolved in methylene chloride
6. 6
   세척washed with water, aqueous sodium bicarbonate and brine
7. 7
   기타After drying
8. 8
   여과(Na2SO4), filtration and concentration in vacuo
9. 9
   기타the crude mixture is chromatographed on silica gel

실험 절차

A mixture of 2-(3-chloro-4-methoxyphenyl)-4-hydroxy-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-4,5-dihydro-1H-imidazole (10 mmol) and p-toluenesulfonic acid monohydrate (1 mmol) in toluene (100 mL) is heated to reflux for 72 hours. The reaction mixture is cooled and the solvent removed under reduced pressure. The crude residue is redissolved in methylene chloride and washed with water, aqueous sodium bicarbonate and brine. After drying (Na2SO4), filtration and concentration in vacuo, the crude mixture is chromatographed on silica gel using toluene/ethyl acetate to give pure 2-(3-chloro-4-methoxyphenyl)-1-[4-(methylsulfonyl)phenyl]-4-trifluoromethyl-1H-imidazole.

출처