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
- 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, prepared as described in Application Example 1, and 9.7 g of N-ethyl-N-(b-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-(b-ethoxycarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.
後処理
- customprepared
- customThe suspension obtained
- temperatureThe reaction mixture is then cooled to approximately 20° C.
- washwashed with 3 times 100 cm3 of water
- 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-17311acfc39048cdb36fc053b4c64d82
- 出典データセット
- uspto-grants-1995_08
- 特許番号
- US05442070
関連ノート
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