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Hydrochloric Acid → 1-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine

HRID 1837748
ノート
印刷プレビュー

反応式

HRID 1837748 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][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[O:18])[CH2:12][CH2:11]2)=[CH:7][CH:6]=[CH:5][N:4]=1.Cl>C(#N)C>[O:2]=[C:3]1[C:8]([CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH2:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[NH:25][S:26]([CH3:29])(=[O:28])=[O:27])=[O:18])[CH2:14][CH2:15]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

4

反応物 2

HCID 313Hydrochloric AcidHCID 226783911-[(2-Methoxy-3-pyridyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine

生成物 1

HCID 226783001-[(2-Oxo-1,2-dihydro-3-pyridinyl)methyl]-4-[2-(2-methylsulfonylaminophenyl)-2-oxoethyl]piperidine収率 51.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

In acetonitrile (4 ml) were dissolved 90 mg of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(2-methanesulfonylaminophenyl)-2-oxoethyl]piperidine obtained in Example 65 and 0.30 ml of concentrated hydrochloric acid, followed by heating under reflux for 5 hours. The solvent was evaporated, and then the residue was dissolved in ethyl acetate and an aqueous 1N sodium hydroxide. The organic layer was separated, washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was recrystallized from ethanol, to give 45 mg of the title compound as colorless crystals.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 5 hours
  3. customThe solvent was evaporated
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. customThe organic layer was separated
  6. washwashed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe solvent was evaporated
  9. customthe crude product was recrystallized from ethanol

出典と根拠

ORDレコード
ord-3209161db6834257a7466943a4a72ec1
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

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