反应详情

温度

-10 °C

To a −60° C. solution of 6-methyl-pyridine-2-carbaldehyde (25 g, 206 mmol) in tetrahydrofuran (200 mL) was added methyl magnesium bromide (200 mL, 1.4 M in tetrahydrofuran/toluene, 1.36 equiv) over 40 minutes. The reaction mixture was slowly warmed to −10° C. over 90 minutes, and then slowly quenched with saturated aqueous ammonium chloride (75 mL). The liquid phase was decanted from the solids and concentrated in vacuo. The resulting residue was dissolved in methylene chloride, dried over magnesium sulfate, and concentrated in vacuo to yield 1-(6-Methyl-pyridin-2-yl)-ethanol (28 g, 100%).

1. customslowly quenched with saturated aqueous ammonium chloride (75 mL)
2. customThe liquid phase was decanted from the solids
3. concentrationconcentrated in vacuo
4. dissolutionThe resulting residue was dissolved in methylene chloride
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo