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

HRID 1870278노트

반응식

HRID 1870278 반응식
[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

참가 물질

4

반응물 3

HCID 1049PyridineHCID 24813Phosphorus oxychlorideHCID 178518984HCID 178518984, 화합물

생성물 1

HCID 135684483,5-Dichloro-1,2-benzoxazole수율 92%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8bc43c0348544deb87d76d9f2f50235c
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06096771

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