반응 #462438

반응 방정식

sodium carbonate

2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline

N-methyl-N-(β-cyanoethyl)amine

→

3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(β-cyanoethyl)amino]quinoline

수율 100.1%

용매

toluene

반응 조건

후처리

1. 1
   기타The suspension obtained
2. 2
   온도is heated
3. 3
   온도to reflux
4. 4
   세척washed with 3 times 50 cm3 of water
5. 5
   농축The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C

실험 절차

19.08 g of sodium carbonate are added to a solution of 16.3 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 10 g of N-methyl-N-(β-cyanoethyl)amine in 160 cm3 of toluene. The suspension obtained is heated to reflux and then stirred for 4 hours at this temperature. The reaction mixture is then cooled to approximately 20° C. and thereafter washed 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-cyanoethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.

출처