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

HRID 232879노트

반응식

HRID 232879 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6a5a64fb2f7e44cf90fd5061572d66b0
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

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