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

HRID 1173122ノート

反応式

HRID 1173122 の反応式
[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

参加物

3

反応物 2

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

生成物 1

HCID 135319672-Chloro-1,6-naphthyridine収率 58.45%

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2f864acd90334f0488ce84625148b9c4
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

反応ノート

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