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Pyridinium chloride → 3-(2-(4,7-Dimethylbenzoxazol-2-yl)ethyl)-5-ethyl-6-methylpyridin-2(1H)-one

HRID 1032998
ノート
印刷プレビュー

反応式

HRID 1032998 の反応式
C[O:2][C:3]1[C:8]([CH2:9][CH2:10][C:11]2[O:12][C:13]3[C:19]([CH3:20])=[CH:18][CH:17]=[C:16]([CH3:21])[C:14]=3[N:15]=2)=[CH:7][C:6]([CH2:22][CH3:23])=[C:5]([CH3:24])[N:4]=1.Cl.N1C=CC=CC=1>O>[CH3:21][C:16]1[C:14]2[N:15]=[C:11]([CH2:10][CH2:9][C:8]3[C:3](=[O:2])[NH:4][C:5]([CH3:24])=[C:6]([CH2:22][CH3:23])[CH:7]=3)[O:12][C:13]=2[C:19]([CH3:20])=[CH:18][CH:17]=1
参加物反応条件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 10176127Pyridinium chlorideHCID 10381616HCID 10381616、化合物

生成物 1

HCID 4534443-(2-(4,7-Dimethylbenzoxazol-2-yl)ethyl)-5-ethyl-6-methylpyridin-2(1H)-one収率 42.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

A mixture of crude 2-methoxy-3-[2-(4,7-dimethylbenzoxazol-2-yl)ethyl]-5-ethyl-6-methylpyridine (161 mg, 0.49 mmol) and pyridine hydrochloride (574 mg, 4.97 mmol) was warmed in a pre-heated oil bath at 140° C. for 15 minutes. The cooled residue was diluted with water and the product extracted into chloroform. This extract was dried (Na2SO4), filtered and the solvent evaporated. This residue was chromatographed on silica gel and eluted with a 0.5 to 2.5% methanol/chloroform gradient to yield 65 mg of pure product. The product was crystallized from diethyl ether to give 38 mg, m.p. 151.5°-153° C.

後処理

  1. extractionthe product extracted into chloroform
  2. dry with materialThis extract was dried (Na2SO4)
  3. filtrationfiltered
  4. customthe solvent evaporated
  5. customThis residue was chromatographed on silica gel
  6. washeluted with a 0.5 to 2.5% methanol/chloroform gradient

出典と根拠

ORDレコード
ord-d3b4f28e98b24e458e904a8098a43d5f
出典データセット
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05308854

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート