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 Hydroxide → 1-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(methylsulfonyl)phenethyl]piperidine

HRID 1837742
ノート
印刷プレビュー

反応式

HRID 1837742 の反応式
C[O:2][C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[S:24]([CH3:27])(=[O:26])=[O:25])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1.S(Cl)(Cl)=O.[OH-].[Na+]>C(O)C>[O:2]=[C:3]1[C:8]([CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[S:24]([CH3:27])(=[O:26])=[O:25])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][NH:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 226785581-[(2-Methoxy-3-pyridyl)methyl]-4-[2-(methylsulfonyl)phenethyl]piperidine

生成物 1

HCID 226787401-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(methylsulfonyl)phenethyl]piperidine収率 79.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

479 mg of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(methylsulfonyl)phenethyl]piperidine obtained in Example 1 and 2 ml of thionyl chloride were dissolved in 50 ml of ethanol, and the mixture was heated under reflux for 2 hours. The reaction mixture was basified by adding a 1N aqueous sodium hydroxide thereto, and the mixture was extracted with dichloromethane. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting crude product was purified by silica gel column chromatography (ethyl acetate), to give 368 mg of the title compound as white crystals.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. extractionthe mixture was extracted with dichloromethane
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated
  7. customthe resulting crude product was purified by silica gel column chromatography (ethyl acetate)

出典と根拠

ORDレコード
ord-74ec9cf3de53440eb6132058cd2eb88e
出典データセット
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06784192B2

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