反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Charged a flask with methyl 2-(4-methylthiazol-2-ylamino)isonicotinate (0.5 g, 2.01 mmol) and added ether (10 mL). The reaction mixture was cooled to 0° C. and diisobutylaluminum hydride (8.01 mL, 8.01 mmol) was added. The reaction mixture was stirred at 0° C. for 8 hours and then stirred overnight at room temperature. The reaction mixture was quenched with water, extracted with ethyl acetate, dried over magnesium sulfate, filtered, and concentrated. The residue was purified using silica gel column chromatography with ethyl acetate as the eluent to afford (2-(4-methylthiazol-2-ylamino)pyridin-4-yl)methanol (0.347 g, 76.6% yield) as white solid. 1H NMR (CD3OD) δ 8.20 (d, 1H), 7.01 (m, 1H), 6.86 (m, 1H), 6.42 (m, 1H), 4.60 (s, 2H), 2.27 (d, 3H); Mass spectrum (apci) m/z=222 (55) (M+H).
WORKUP
后处理
- stirringstirred overnight at room temperature
- customThe reaction mixture was quenched with water
- extractionextracted with ethyl acetate
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified