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

HRID 375251
ノート
印刷プレビュー

反応式

HRID 375251 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.[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]
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

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7d8803ae8c124ed0a26fc4057abaa942
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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