تفاعل #59014

ord-458d9a1e8645405eb676b540a297368a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07423185B2uspto-grants-2008_09