تفاعل #48544

ord-9930678f962847d1aa3e1e730e0a3dbf

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled to between 10 and 15° C
  2. 2
    تركيزconcentrated under reduced pressure
  3. 3
    workup.ADDITIONThe residue was diluted with ether
  4. 4
    غسيلthe solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine
  5. 5
    تجفيفIt was then dried over MgSO4
  6. 6
    أخرىevaporated under reduced pressure

الإجراء التجريبي

A solution of ethyl isonipecotate (27.6 g, 175 mmol) in dichloromethane (50 ml) was added dropwise over 10 minutes to a solution of 3-chlorobenzoyl chloride (20 ml, 160 mmol) and triethylamine (28 ml, 200 mmol) in dichloromethane (500 ml) cooled to between 10 and 15° C. The reaction was then stirred at room temperature for 3 hours and concentrated under reduced pressure. The residue was diluted with ether, the solution washed with 1N hydrochloric acid, sodium carbonate solution (×3) and brine. It was then dried over MgSO4 and evaporated under reduced pressure, to give the title compound as a solid, 44.49.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745630B2uspto-grants-2010_06