تفاعل #84552

ord-aa565b51f54e4f788b914aab720434e4

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed overnight
  2. 2
    استخلاصThe resulting mixture was extracted with DCM (40 mL×2)
  3. 3
    غسيلThe combined organic phases were washed with brine (40 mL×2)
  4. 4
    تجفيفdried over anhydrous Na2SO4
  5. 5
    تركيزconcentrated in vacuo
  6. 6
    أخرىThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1)

الإجراء التجريبي

A mixture of 3-fluorophenol (3.36 g, 30.0 mmol), ethyl 2-bromo-2-methylpropanoate (8.78 g, 45.0 mmol) and K2CO3 (6.22 g, 45.0 mmol) in acetone (50 mL) was refluxed overnight. The mixture was cooled to rt and 60 mL of water was added. The resulting mixture was extracted with DCM (40 mL×2). The combined organic phases were washed with brine (40 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=4:1) to give the title compound as colorless liquid (3.20 g, 47%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434695B2uspto-grants-2016_09