HRID2278169
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
A round bottom flask was charged with di(pyridin-3-yl)methanone (500 mg, 2.72 mmol), MeOH (30 mL), and CH2Cl2 (15 mL) and cooled to 0° C. NaBH4 (51 mg, 1.35 mmol) was added in one portion. The solution was stirred for 1 h at 0° C. and quenched with 1N NaOH and the reaction was extracted with CH2Cl2 (3×). The organic layers were combined, dried over Na2SO4 and concentrated under reduced pressure. Crude di(pyridin-3-yl)methanol (505 mg, 100%) was used in the next step without further purification. 1H NMR 400 MHz (CDCl3) δ 8.32 (s, 2H), 8.24 (d, J=4.8 Hz, 2H), 7.47 (d, J=7.9 Hz, 2H), 7.09-7.01 (m, 2H), 5.67 (s, 1H).
WORKUP
后处理
- customquenched with 1N NaOH
- extractionthe reaction was extracted with CH2Cl2 (3×)
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customCrude di(pyridin-3-yl)methanol (505 mg, 100%) was used in the next step without further purification