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

HRID 1032998
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HRID 1032998 반응식
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
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참가 물질

4

반응물 2

HCID 10176127Pyridinium chlorideHCID 10381616HCID 10381616, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
140 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d3b4f28e98b24e458e904a8098a43d5f
출처 데이터셋
uspto-grants-1994_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05308854

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