반응 #59014

반응 방정식

hydrochloric acid

Trifluoromethanesulfonic anhydride

4-bromo-2-isopropylphenol

pyridine

→

4-bromo-2-isopropylphenyl methanesulfonate

용매

ethyl acetate

methylene chloride

반응 조건

후처리

1. 1
   온도cooled
2. 2
   workup.STIRRINGThe mixture was stirred for 10 min
3. 3
   기타The organic layer was separated
4. 4
   세척washed with water and brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   기타The solvent was evaporated under reduced pressure
7. 7
   기타the residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/10)

실험 절차

Trifluoromethanesulfonic anhydride (0.47 mL) was added to an ice-cooled mixture of 4-bromo-2-isopropylphenol (0.5 g) and pyridine (0.28 mL) in methylene chloride (5 mL) with stirring. The mixture was stirred for 10 min, and poured into a mixture of ethyl acetate and 1 mol/L hydrochloric acid. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/10) to afford 4-bromo-2-isopropylphenyl methanesulfonate (0.71 g).

출처