HRID1174112
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
- 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
- customwas flushed with nitrogen
- additiontreated with water (5 mL), ammonium formate (2.5 g) and Pd/C (1.0 g)
- temperatureThe reaction mixture was cooled
- filtrationfiltered
- concentrationconcentrated
- washA solution of the residue in dichloromethane (100 mL) was washed with saturated aqueous NaHCO3 (3×50 mL)
- concentrationThe isolated dichlormethane layer was concentrated