HRID2407800

反应详情

EQUATION

反应方程式

HRID 2407800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl 3′-formylbiphenyl-4-carboxylate (0.338 g) was dissolved in 2 mol/L dimethylamine in tetrahydrofuran (20 mL) and stirred at room temperature for 1 hour. Sodium triacetoxyborohydride (0.895 g) was added. The reaction was stirred at room temperature for 5 days and then partitioned between saturated aqueous sodium bicarbonate and ethyl acetate. The organics were dried over magnesium sulfate and concentrated under reduced pressure to afford the crude material, which was purified by flash column chromatography (eluant: 0-5% methanol/dichloromethane (0.5% triethylamine) to furnish the title compound (0.112 g) having the following physical data.

WORKUP

后处理

  1. stirringThe reaction was stirred at room temperature for 5 days
  2. custompartitioned between saturated aqueous sodium bicarbonate and ethyl acetate
  3. dry with materialThe organics were dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto afford the crude material, which
  6. customwas purified by flash column chromatography (eluant