تفاعل #343763

ord-f14a8b62c6884870a484f598b5c82ebb

ظروف التفاعل

درجة الحرارة
110°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter removal of the (-)-menthol under reduced pressure
  2. 2
    أخرىthe residue was chromatographed on silica gel
  3. 3
    workup.ADDITIONFractions containing the title compound
  4. 4
    أخرىevaporated under reduced pressure

الإجراء التجريبي

To a mixture of 2-(pyrrol-1-yl)malonic acid diethyl ester (300.0 g) and (-)-menthol (417.0 g) was added tetraethyl titanate (10.0 g), and the resulting mixture was stirred at 110° C. for 19 hours. After removal of the (-)-menthol under reduced pressure, the residue was chromatographed on silica gel using n-hexane/ethyl acetate (50:1) as the eluent. Fractions containing the title compound were pooled and evaporated under reduced pressure to give the title compound (142.0 g, 31.8%) as a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05258382uspto-grants-1993_11