Ethyl 2-methylnicotinate → (2-Methylpyridin-3-yl)methanol
반응식
[CH3:1][C:2]1[N:12]=[CH:11][CH:10]=[CH:9][C:3]=1[C:4](OCC)=[O:5].[H-].C([Al+]CC(C)C)C(C)C>ClCCl>[CH3:1][C:2]1[C:3]([CH2:4][OH:5])=[CH:9][CH:10]=[CH:11][N:12]=1참가 물질
4
실험 절차
Ethyl 2-methylnicotinate 18-1 (257 mg) was mixed with dichloromethane (4 ml) and to the mixture at −78° C. was added dropwise 1 M diisobutyl aluminium hydride (4 ml), followed by siring for 1 hour. The reaction was quenched with methanol and to the mixture was added aqueous Rochel solution (20 ml), followed by stirring for 2 hours. The resulting mixture was extracted with dichloromethane, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was column-chromatographed (ethyl acetate/hexane=1/1) to yield the compound 18-2 (166 mg, 87%).
후처리
- customThe reaction was quenched with methanol and to the mixture
- additionwas added aqueous Rochel solution (20 ml)
- extractionThe resulting mixture was extracted with dichloromethane
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was column-chromatographed (ethyl acetate/hexane=1/1)
출처 및 근거
- ORD 기록
- ord-5653aa90a8324e35aa41e36d14158de6
- 출처 데이터셋
- uspto-grants-2011_12
- 특허 번호
- US08071650B2
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