Aluminium lithium hydride → (2-Ethylpyridin-3-yl)methanol
反応式
[Li+].[CH2:2]([C:4]1[N:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([O-])=[O:7])[CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH2:2]([C:4]1[C:5]([CH2:6][OH:7])=[CH:9][CH:10]=[CH:11][N:12]=1)[CH3:3]参加物
4
実験手順
The 2-ethyl nicotinic acid lithium salt (5 g, 3.18 mmol) in distilled THF (400 mL) under nitrogen was cooled to 0° C. and lithium aluminum hydride (1M in THF) (25 mL) was added dropwise. The reaction was stirred for 3 hours at room temperature then cooled to 0° C. and quenched with EtOAc (949 μL), then H2O (949 μL), then 15% NaOH (949 μL), followed by H2O (2.8 mL). The solution was filtered and the solvent removed under reduced pressure. Toluene was added and the solvent was removed under reduced pressure to give the desired 2-ethyl-3 -hydroxymethylpyridine.
後処理
- temperaturethen cooled to 0° C.
- customquenched with EtOAc (949 μL)
- filtrationThe solution was filtered
- customthe solvent removed under reduced pressure
- additionToluene was added
- customthe solvent was removed under reduced pressure
出典と根拠
- ORDレコード
- ord-aaa0ddfbf41e452299afe064a36ec3cd
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05726172
反応ノート
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