Methyl 5-fluoro-2-methoxynicotinate → (5-Fluoro-2-methoxypyridin-3-yl)methanol
반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[N:6][C:5]=1[O:11][CH3:12].[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[F:10][C:8]1[CH:9]=[C:4]([CH2:3][OH:2])[C:5]([O:11][CH3:12])=[N:6][CH:7]=1참가 물질
4
실험 절차
To 5-fluoro-2-methoxy-nicotinic acid methyl ester (35, 10 g, 54.0 mmol) in 200 mL of tetrahydrofuran, lithium aluminum hydride (81 mL, 1 M in tetrahydrofuran, 81 mmol) was added dropwise at −78° C. and stirred for several hours. The reaction was quenched with dropwise addition of 3 mL water, 3 mL of 15% aqueous sodium hydroxide, and 10 mL of water sequentially, then 200 mL of methyl t-butyl ether was added. Solids were filtered out and the filtrate concentrated under vacuum to provide the desired compound as a white solid (36, 8 g, 50.9 mmol, 94%).
후처리
- customThe reaction was quenched with dropwise addition of 3 mL water, 3 mL of 15% aqueous sodium hydroxide, and 10 mL of water sequentially
- addition200 mL of methyl t-butyl ether was added
- filtrationSolids were filtered out
- concentrationthe filtrate concentrated under vacuum
출처 및 근거
- ORD 기록
- ord-b29179959d2949238ba087f904f9435b
- 출처 데이터셋
- uspto-grants-2015_08
- 특허 번호
- US09096593B2
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