HRID2278169

反应详情

EQUATION

反应方程式

HRID 2278169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customquenched with 1N NaOH
  2. extractionthe reaction was extracted with CH2Cl2 (3×)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customCrude di(pyridin-3-yl)methanol (505 mg, 100%) was used in the next step without further purification