Pyridine → 3,5-Dichloro-1,2-benzoxazole

HRID 1870278ノート

反応式

HRID 1870278 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7](O)[C:6]=2[CH:11]=1.N1C=CC=CC=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:7]1[C:6]2[CH:11]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1

参加物

4

反応物 3

HCID 1049PyridineHCID 24813Phosphorus oxychlorideHCID 178518984HCID 178518984、化合物

生成物 1

HCID 135684483,5-Dichloro-1,2-benzoxazole収率 92%

実験手順

To a suspension of 5-chloro-3-hydroxy-1,2-benzisoxazole (100 g) in phosphorus oxychloride (80 ml) was added pyridine (48 ml) dropwise over 1 hours with stirring at room temperature, and the mixture was then refluxed for 5 hours. The reaction mixture was added to ice water (500 ml) and extracted with ethyl acetate and the combined extracts were dried over anhydrous magnesium sulphate. The solvent was evaporated under reduced pressure and the title compound (102 g, 92%) was obtained by recrystallizing the residue from petroleum ether as a colorless needle.

後処理

  1. temperaturethe mixture was then refluxed for 5 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialthe combined extracts were dried over anhydrous magnesium sulphate
  4. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-8bc43c0348544deb87d76d9f2f50235c
出典データセット
uspto-grants-2000_08
特許番号
US06096771

反応ノート

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