Sodium Hydroxide → 2-(7-Chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine

HRID 232879ノート

反応式

HRID 232879 の反応式
P(Cl)(Cl)(Cl)=O.[C:6]([CH2:9][CH2:10][S:11][CH:12]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[CH2:16][O:15][C:14]2[CH:23]=[CH:24][C:25]([O:27][CH2:28][C:29]3[CH:38]=[CH:37][C:36]4[C:31](=[CH:32][C:33]([Cl:39])=[CH:34][CH:35]=4)[N:30]=3)=[CH:26][C:13]1=2)(=O)[NH2:7].[OH-].[Na+]>CN(C)C=O>[Cl:39][C:33]1[CH:32]=[C:31]2[C:36]([CH:37]=[CH:38][C:29]([CH2:28][O:27][C:25]3[CH:24]=[CH:23][C:14]4[O:15][CH2:16][C:17]5[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=5[CH:12]([S:11][CH2:10][CH2:9][C:6]#[N:7])[C:13]=4[CH:26]=3)=[N:30]2)=[CH:35][CH:34]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 2335915311-(2-Carbamoylethylthio)-2-(7-chloroquinolin-2-yl)methoxy-6,11-dihydrodibenz[b,e]oxepine

生成物 1

HCID 233591442-(7-Chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Under ice cooling and stirring, 1.35 ml of phosphorus oxy-chloride was added dropwise over 40 minutes to 1.78 g of 11-(2-carbamoylethylthio)-2-(7-chloroquinolin-2-yl)methoxy-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 63 dissolved in 14 ml of dimethylformamide and the mixture was stirred at the same temperature for 30 minutes. The reaction mixture was added 250 ml of a 1% sodium hydroxide aqueous solution, crystals precipitated were collected by filtration and the crystals were dissolved in chloroform. After this chloroform solution was washed with water and dried over anhydrous sodium sulfate, the solvent was removed to obtain 1.62 g of the title compound.

後処理

  1. customobtained in Reference example 63
  2. stirringthe mixture was stirred at the same temperature for 30 minutes
  3. customprecipitated
  4. filtrationwere collected by filtration
  5. dissolutionthe crystals were dissolved in chloroform
  6. washAfter this chloroform solution was washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customthe solvent was removed

出典と根拠

ORDレコード
ord-6a5a64fb2f7e44cf90fd5061572d66b0
出典データセット
uspto-grants-1997_01
特許番号
US05591752

反応ノート

読み込み中…