반응식
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.C.[ClH:10]>CO>[Cl:10][C:7]1[C:2]([OH:1])=[CH:3][CH:4]=[C:5]([CH3:8])[N:6]=1참가 물질
5
실험 절차
5-Hydroxy-2-methylpyridine (1-014-01) (27.01 g) was dissolved in conc. hydrochloric acid (200 mL) and to the reaction mixture was bubbled chlorine gass at 68 to 74° C. After the reaction mixture was stood overnight, the volatile was removed by bubbling nitrogen gas. The reaction mixture was evaporated under reduced pressure to give the crystal residue. The crystal residue was dissolved in methanol, and treated with active charcoal. After recrystallization, the desired 2-chloro-3-hyroxy-6-methylpyridine (1-014-02) (23.96 g, 67.3%) was obtained.
후처리
- customwas bubbled chlorine gass at 68 to 74° C
- customthe volatile was removed
- customby bubbling nitrogen gas
- customThe reaction mixture was evaporated under reduced pressure
- customto give the crystal residue
- customAfter recrystallization
출처 및 근거
- ORD 기록
- ord-2b07074f87f74c3fa762d2f57ac48cfd
- 출처 데이터셋
- uspto-grants-2005_12
- 특허 번호
- US06977266B2
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