Phosphorus oxychloride → HCID 18674967、化合物

HRID 1634886

反応式

HRID 1634886 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH3:6][O:7][C:8]1[CH:9]=[C:10]([C:18]2[CH:23]=[CH:22][N+:21]([O-])=[CH:20][CH:19]=2)[CH:11]=[C:12]([O:16][CH3:17])[C:13]=1[O:14][CH3:15]>>[Cl:3][C:22]1[CH:23]=[C:18]([C:10]2[CH:9]=[C:8]([O:7][CH3:6])[C:13]([O:14][CH3:15])=[C:12]([O:16][CH3:17])[CH:11]=2)[CH:19]=[CH:20][N:21]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 186750144-(3,4,5-Trimethoxyphenyl)pyridine-N-oxide

生成物 1

HCID 18674967HCID 18674967、化合物

反応条件

温度
100 °C

実験手順

Phosphorus oxychloride (2 mL) was added to 4-(3,4,5-Trimethoxyphenyl)pyridine-N-oxide (27 mg) at 0° C., and the mixture was stirred at 100° C. for 5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate and neutralized with a saturated aqueous solution of sodium hydrogencarbonate at 0° C. The neutralized product was extracted with ethyl acetate, and the extract was washed with saturated brine and dried over anhydrous sodium sulfate. The residue was purified by column chromatography on silica gel (ethyl acetate) to obtain the title compound.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionthe residue was diluted with ethyl acetate
  3. customneutralized with a saturated aqueous solution of sodium hydrogencarbonate at 0° C
  4. extractionThe neutralized product was extracted with ethyl acetate
  5. washthe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe residue was purified by column chromatography on silica gel (ethyl acetate)

出典と根拠

ORDレコード
ord-62f8bfb40c614624866584b26b49cb17
出典データセット
uspto-grants-2003_01
特許番号
US06509329B1

関連ノート

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