Sodium Carbonate → 3-ethoxycarbonyl-6,7-difluoro-2-[N-ethyl N-(beta-ethoxycarbonylethyl)amino]quinoline

HRID 375251

반응식

HRID 375251 반응식
C(=O)([O-])[O-].[Na+].[Na+].Cl[C:8]1[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:16][C:15]2[C:10](=[CH:11][C:12]([F:24])=[C:13]([F:23])[CH:14]=2)[N:9]=1.[CH2:25]([NH:27][CH2:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])[CH3:26]>C1(C)C=CC=CC=1>[CH2:21]([O:20][C:18]([C:17]1[C:8]([N:27]([CH2:25][CH3:26])[CH2:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[N:9][C:10]2[C:15]([CH:16]=1)=[CH:14][C:13]([F:23])=[C:12]([F:24])[CH:11]=2)=[O:19])[CH3:22]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 90223Ethyl N-ethyl-beta-alaninateHCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinoline

생성물 1

HCID 98428373-ethoxycarbonyl-6,7-difluoro-2-[N-ethyl N-(beta-ethoxycarbonylethyl)amino]quinoline수율 92.8%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
90 °C

실험 절차

7.8 g of sodium carbonate are added to a solution of 10 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 9.7 g of N-ethyl-N-(β-ethoxycarbonylethyl)amine in 120 cm3 of toluene. The suspension obtained is heated to approximately 90° C. 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 100 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 13 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-ethyl-N-(β-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent step.

후처리

  1. customThe suspension obtained
  2. temperatureThe reaction mixture is then cooled to approximately 20° C.
  3. washwashed with 3 times 100 cm3 of water
  4. concentrationThe organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C

출처 및 근거

ORD 기록
ord-7d8803ae8c124ed0a26fc4057abaa942
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484921

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