Sodium Carbonate → 3-ethoxycarbonyl-6,7-difluoro-2-(N-methyl-N-beta-cyanoethylamino)quinoline

HRID 1756801

反応式

HRID 1756801 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]#[N: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]#[N: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 69656Propanenitrile, 3-(methylamino)-HCID 97954612-Chloro-3-ethoxycarbonyl-6,7-difluoroquinoline

生成物 1

HCID 189946093-ethoxycarbonyl-6,7-difluoro-2-(N-methyl-N-beta-cyanoethylamino)quinoline収率 100.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
20 °C

実験手順

19.08 g of sodium carbonate are added to a solution of 16.3 g of 2-chloro-3-ethoxycarbonyl-6,7-difluoroquinoline, prepared as described in Application Example 1, and 10 g of N-methyl-N-(b-cyanoethyl)amine in 160 cm3 of toluene. The suspension obtained is heated to reflux 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 50 cm3 of water. The organic phase is concentrated to dryness under reduced pressure (20 kPa) at approximately 50° C. 19.17 g of 3-ethoxycarbonyl-6,7-difluoro-2-[N-methyl-N-(b-cyanoethyl)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 50 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-ddc358b655004cd0aad3ab7f54f7f839
出典データセット
uspto-grants-1995_08
特許番号
US05442070

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