Phosphorus oxychloride → 2-Chloro-1,6-naphthyridine

HRID 1173122노트

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HRID 1173122 반응식
[NH:1]1[C:10]2[C:5](=[CH:6][N:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]1=O.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:2]1[CH:3]=[CH:4][C:5]2[C:10](=[CH:9][CH:8]=[N:7][CH:6]=2)[N:1]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 5896741,6-Naphthyridin-2(1H)-One

생성물 1

HCID 135319672-Chloro-1,6-naphthyridine수율 58.45%

반응 조건

온도
120 °C

실험 절차

1,6-Naphthyridine-2-one (1.0 g, J. Org. Chem. 4744 (1990)) was dissolved in phosphorous oxychloride (19 ml), followed by heating under reflux at 120° C. for 2 hours. After cooling, the solvent was evaporated, and the residue was basified with water and potassium carbonate. Then, the mixture was extracted with ethyl acetate, and the extract was washed with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, to give the title compound (0.658 g, 58.45%) as orange crystals.

후처리

  1. temperatureby heating
  2. temperatureAfter cooling
  3. customthe solvent was evaporated
  4. extractionThen, the mixture was extracted with ethyl acetate
  5. washthe extract was washed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated

출처 및 근거

ORD 기록
ord-2f864acd90334f0488ce84625148b9c4
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834049B2

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