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

HRID 375246

반응식

HRID 375246 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.[CH3:25][NH:26][CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30]>C1(C)C=CC=CC=1>[CH2:21]([O:20][C:18]([C:17]1[C:8]([N:26]([CH3:25])[CH2:27][CH2:28][C:29]([O:31][CH2:32][CH3:33])=[O:30])=[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 541480Ethyl 3-(methylamino)propanoateHCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinoline

생성물 1

HCID 117282483-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(beta-ethoxycarbonylethyl)amino]quinoline수율 96.8%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
90 °C

실험 절차

56.2 g of sodium carbonate are added to a solution of 72 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 45.1 g of N-methyl-N-(β-ethoxycarbonylethyl)amine in 750 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 400 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 94 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(β-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.

후처리

  1. customThe suspension obtained
  2. temperatureThe reaction mixture is then cooled to approximately 20° C.
  3. washwashed with 3 times 400 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-3b64b8e9434246f085527a6f09a497b7
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484921

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