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alpha-(5-Ethyl-2-methoxy-6-methyl-3-pyridinyl)-2-benzoxazoleethanol → 3-[2-(benzoxazol-2-yl)ethenyl]-5-ethyl-6-methyl-2-(1H)-pyridinone

HRID 1590028
ノート
印刷プレビュー

反応式

HRID 1590028 の反応式
O[CH:2]([C:13]1[C:14]([O:22]C)=[N:15][C:16]([CH3:21])=[C:17]([CH2:19][CH3:20])[CH:18]=1)[CH2:3][C:4]1[O:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[N:8]=1.Cl.N1C=CC=CC=1>>[O:5]1[C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[N:8]=[C:4]1[CH:3]=[CH:2][C:13]1[C:14](=[O:22])[NH:15][C:16]([CH3:21])=[C:17]([CH2:19][CH3:20])[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 10064107alpha-(5-Ethyl-2-methoxy-6-methyl-3-pyridinyl)-2-benzoxazoleethanolHCID 10176127Pyridinium chloride

生成物 1

HCID 4548263-[2-(benzoxazol-2-yl)ethenyl]-5-ethyl-6-methyl-2-(1H)-pyridinone収率 76%

実験手順

A mixture of 2-[2(R/S)-hydroxy-2-(2-methoxy-5-ethyl-6-methylpyridin-3-yl)ethyl]benzoxazole (72 mg, 0.23 mmol) and pyridine hydrochloride (133 mg, 1.2 mmol), under a nitrogen atmosphere, was placed in a preheated oil bath (165° C.) for 5 minutes. The reaction flask was removed, cooled, and water added to give a solid. This crude product was extracted into chloroform, dried (MgSO4) and the solvent evaporated to yield 49 mg (75%) of pure product. Recrystallization from methanol gave 15 mg of analytically pure product, mp 262°-264° C.

後処理

  1. customunder a nitrogen atmosphere, was placed in a preheated oil bath
  • customThe reaction flask was removed
  • temperaturecooled
  • additionwater added
  • customto give a solid
  • extractionThis crude product was extracted into chloroform
  • dry with materialdried (MgSO4)
  • customthe solvent evaporated
  • 出典と根拠

    ORDレコード
    ord-5abc988ee7f245cd99eeb447e23a803a
    出典データセット
    uspto-grants-1993_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US05202243

    反応ノート

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