Water → HCID 178483250、化合物

HRID 1985874ノート

反応式

HRID 1985874 の反応式
C([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:6](=[C:14](OC)[C:15]2[CH:20]=[CH:19][CH:18]=[C:17](I)[CH:16]=2)[C:5]1=[O:24])(=O)C.[CH3:25][N:26]([CH2:28][C:29]1[CH:35]=[CH:34][C:32]([NH2:33])=[CH:31][CH:30]=1)[CH3:27].[OH-].[Na+].O.[CH3:39][N:40](C)C=O>>[CH3:27][N:26]([CH2:28][C:29]1[CH:35]=[CH:34][C:32]([NH:33]/[C:14](=[C:6]2\[C:5](=[O:24])[NH:4][C:12]3[C:7]\2=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=3)/[C:15]2[CH:16]=[CH:17][C:18]([C:39]#[N:40])=[CH:19][CH:20]=2)=[CH:31][CH:30]=1)[CH3:25]

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 308051Benzenemethanamine, 4-amino-N,N-dimethyl-HCID 68676237HCID 68676237、化合物2 回

生成物 1

HCID 178483250HCID 178483250、化合物

反応条件

温度
80 °C

実験手順

1.07 g of 1-acetyl-3-[1-chloro-1-(4-cyanophenyl)methylene]-6-chloro-2-indolinone (starting material VII) and 0.54 g of 4-(dimethylaminomethyl)aniline (starting material IX.4) are dissolved in 10 ml of dimethylformamide and stirred at 80° C. for 3 hours. After cooling, 1 ml of 6N aqueous sodium hydroxide is added, and the mixture is stirred at room temperature for 30 minutes. Water is added and the mixture is extracted three times with methylene chloride. The combined organic phases are washed twice with water, dried over sodium sulphate and concentrated using a rotary evaporator, and the product is recrystallized from diethyl ether.

後処理

  1. temperatureAfter cooling
  2. stirringthe mixture is stirred at room temperature for 30 minutes
  3. extractionthe mixture is extracted three times with methylene chloride
  4. washThe combined organic phases are washed twice with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. customa rotary evaporator
  8. customthe product is recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-09c54c4d7fd64222961121a1417d86ae
出典データセット
uspto-grants-2009_06
特許番号
US07547703B2

反応ノート

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