Thionyl Chloride → 2-(Chloromethyl)-6-methylpyridine
반응식
[CH3:1][C:2]1[N:7]=[C:6]([CH2:8]O)[CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:12])=O>C(Cl)Cl>[Cl:12][CH2:8][C:6]1[CH:5]=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1참가 물질
4
실험 절차
A solution of (6-methyl-pyridin-2-yl)-methanol (1.44 g, 11.7 mmol), thionyl chloride (1.45 mL, 19.9 mmol) and methylene chloride (20 mL) was stirred under reflux for 40 minutes. The reaction solution was cooled to room temperature and then concentrated under a reduced pressure. The residue was partitioned into sodium bicarbonate solution and diethyl ether. The organic layer was concentrated under a reduced pressure, and the residue was purified by silica gel chromatography (ethyl acetate) to obtain the title compound (1.42 g, 85.8%).
후처리
- temperatureunder reflux for 40 minutes
- concentrationconcentrated under a reduced pressure
- customThe residue was partitioned into sodium bicarbonate solution and diethyl ether
- concentrationThe organic layer was concentrated under a reduced pressure
- customthe residue was purified by silica gel chromatography (ethyl acetate)
출처 및 근거
- ORD 기록
- ord-78e6bd01107849bd8231580d44d84968
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08841327B2
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