تفاعل #83633

ord-d3b32fb5febb44cbb0481d07d5a8d74a

المذيبات

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe suspension obtained
  2. 2
    درجة الحرارةis heated
  3. 3
    درجة الحرارةat reflux
  4. 4
    غسيلby washing with 3 times 50 cm3 of water
  5. 5
    تركيزThe organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C

الإجراء التجريبي

To a solution of 16.3 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline prepared as described in Example 1 and 10 g of N-methyl-N-β-cyanoethylamine in 160 cm3 of toluene are added 19.08 g of sodium carbonate. The suspension obtained is heated at reflux and then stirred for 4 hours at this temperature. The reaction mixture is subsequently cooled to approximately 20° C., followed by washing with 3 times 50 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 19.17 g of 3-ethoxycarbonyl-6,7-difluoro-2-(N-methyl-N-β-cyanoethylamino)quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05624933uspto-grants-1997_04