HRID1174112

反应详情

EQUATION

反应方程式

HRID 1174112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of the product of Example 2-2 (3.8 g) in methanol (65 mL) in a three-necked round bottom flask equipped with a condenser was flushed with nitrogen, treated with water (5 mL), ammonium formate (2.5 g) and Pd/C (1.0 g), and stirred under nitrogen at 60° C. for 12 hours. The reaction mixture was cooled, filtered, and concentrated. A solution of the residue in dichloromethane (100 mL) was washed with saturated aqueous NaHCO3 (3×50 mL). The isolated dichlormethane layer was concentrated to afford 3.3 g of the crude product.

WORKUP

后处理

  1. customwas flushed with nitrogen
  2. additiontreated with water (5 mL), ammonium formate (2.5 g) and Pd/C (1.0 g)
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. concentrationconcentrated
  6. washA solution of the residue in dichloromethane (100 mL) was washed with saturated aqueous NaHCO3 (3×50 mL)
  7. concentrationThe isolated dichlormethane layer was concentrated