ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium hydride → 2-((2-(Dimethylamino)-2-methylpropyl)thio)-3-phenylquinoline hydrochloride

HRID 1903238
ノート
印刷プレビュー

反応式

HRID 1903238 の反応式
[C:1]1([C:7]2[C:8](=[S:17])[NH:9][C:10]3[C:15]([CH:16]=2)=[CH:14][CH:13]=[CH:12][CH:11]=3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[Na+].[H][H].Cl.[Cl:23][CH2:24][C:25]([N:28]([CH3:30])[CH3:29])([CH3:27])[CH3:26]>CN(C)C=O>[ClH:23].[CH3:29][N:28]([CH3:30])[C:25]([CH3:27])([CH3:26])[CH2:24][S:17][C:8]1[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)=[CH:16][C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[N:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 132002063-Phenylquinolin-2-thioneHCID 227322711-Chloro-2-dimethylamino-2-methylpropane hydrochlorideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 98858482-((2-(Dimethylamino)-2-methylpropyl)thio)-3-phenylquinoline hydrochloride

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

3-Phenylquinolin-2-thione (1.4 g.) was added to a suspension of sodium hydride (0.68 g. of a 50% w/w dispersion in mineral oil) in dimethylformamide (10 ml.) at 0°-5°. When all the hydrogen had evolved, a slurry of 1-chloro-2-dimethylamino-2-methylpropane hydrochloride (1.1 g.) in dimethylformamide (10 ml.) was added and the mixture was stirred at ambient temperature for 20 hr. The mixture was then poured into ice-water (100 ml.) and extracted with ethyl acetate (3×30 ml.). The ethyl acetate extract was washed with brine (30 ml.) and then dried (MgSO4). The solvent was evaporated and the residual oil was chromatographed on basic alumina (125 g., Brockmann Grade III), eluted with increasing concentrations of methylene dichloride in petroleum ether. The eluate obtained with 10% v/v methylene dichloride in petroleum ether was evaporated, the residual oil was dissolved in diethyl ether (20 ml.), and ethereal hydrogen chloride was added until precipitation was complete. The mixture was filtered and the solid residue was crystallised from ethyl acetate to give 2-(2-dimethylamino-2-methylpropylthio)-3-phenylquinoline hydrochloride, m.p. 199°-201°.

後処理

  1. customat 0°-5°
  2. extractionextracted with ethyl acetate (3×30 ml.)
  3. extractionThe ethyl acetate extract
  4. washwas washed with brine (30 ml.)
  5. dry with materialdried (MgSO4)
  6. customThe solvent was evaporated
  7. customthe residual oil was chromatographed on basic alumina (125 g., Brockmann Grade III)
  8. washeluted
  9. temperaturewith increasing concentrations of methylene dichloride in petroleum ether
  10. customThe eluate obtained with 10% v/v methylene dichloride in petroleum ether
  11. customwas evaporated
  12. dissolutionthe residual oil was dissolved in diethyl ether (20 ml.)
  13. additionethereal hydrogen chloride was added until precipitation
  14. filtrationThe mixture was filtered
  15. customthe solid residue was crystallised from ethyl acetate

出典と根拠

ORDレコード
ord-9d6cef58928841afb6486511a00970c1
出典データセット
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04435405

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート