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Water → 3-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(beta-ethoxycarbonylethyl)amino]quinoline

HRID 375254
ノート
印刷プレビュー

反応式

HRID 375254 の反応式
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.[CH:25]1([NH:28][CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])[CH2:27][CH2:26]1.O>C1(C)C=CC=CC=1.C(O)(=O)C>[CH2:21]([O:20][C:18]([C:17]1[C:8]([N:28]([CH:25]2[CH2:26][CH2:27]2)[CH2:29][CH2:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])=[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinolineHCID 13456042Ethyl 3-(cyclopropylamino)propanoate

生成物 1

HCID 189945853-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(beta-ethoxycarbonylethyl)amino]quinoline収率 65.6%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 1140Toluene溶媒

反応条件

温度
20 °C

実験手順

3 g of sodium carbonate are added to a solution of 3.48 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline and 3 g of N-cyclopropyl-N-(β-ethoxycarbonylethyl)amine in 10 cm3 of toluene. The suspension obtained is heated to reflux and then stirred for 15 hours at this temperature. The reaction mixture is then cooled to approximately 20° C. and 30 cm3 of water and 4.5 cm3 of acetic acid are thereafter added. After settling has taken place, the reaction mixture is separated and washed with twice 10 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 3.3 g of crude 3-ethoxycarbonyl-6,7-difluoro-2-[N-cyclopropyl-N-(β-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent step.

後処理

  1. customThe suspension obtained
  2. temperatureis heated
  3. temperatureto reflux
  4. customthe reaction mixture is separated
  5. washwashed with twice 10 cm3 of water
  6. concentrationThe organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C

出典と根拠

ORDレコード
ord-b734297800dd43688690a6e9911a857b
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05484921

反応ノート

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