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

HRID 1756805ノート

反応式

HRID 1756805 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.[CH3:25][NH:26][CH2:27][CH2:28][C:29]([NH2:31])=[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]([NH2:31])=[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]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinolineHCID 22182162N~3~-Methyl-beta-alaninamide

生成物 1

HCID 189945873-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(beta-aminocarbonylethyl)amino]quinoline収率 94.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
20 °C

実験手順

4.4 g of sodium carbonate are added to a solution of 4 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoro-quinoline, prepared as described in Application Example 1, and 3 g of N-methyl-N-(b-aminocarbonylethyl)amine in 40 cm3 of toluene. The suspension obtained is heated to reflux and then stirred for 2 hours 30 minutes at this temperature. The reaction mixture is then cooled to approximately 20° C. and thereafter washed with 3 times 25 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 4.7 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(b-aminocarbonylethyl)amino]quinoline are obtained in the form of an oil, which is used without further purification for the subsequent steps.

後処理

  1. customprepared
  2. customThe suspension obtained
  3. temperatureis heated
  4. temperatureto reflux
  5. washwashed with 3 times 25 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-7708ac1b21994a70812b71fec0d6b38f
出典データセット
uspto-grants-1995_08
特許番号
US05442070

反応ノート

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