Phosphorus oxychloride → HCID 18674967, 화합물

HRID 1634886

반응식

HRID 1634886 반응식
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

참가 물질

3

반응물 2

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

생성물 1

HCID 18674967HCID 18674967, 화합물

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-62f8bfb40c614624866584b26b49cb17
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06509329B1

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