HRID2246530
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
PROCEDURE
实验过程
A solution of Compound 3 (100 mg) and benzylamine (70 μL) in acetonitrile (2 mL) was heated at 110° C. over 8 hours. Solvent was removed under reduced pressure and the crude product was stirred in trifluoroacetic acid (1 mL) for 2 hours at room temperature. Finally, trifluoroacetic acid was removed under reduced pressure and the crude product was partitioned between chloroform (20 mL) and 7% aqueous NaHCO3 solution (10 mL). The chloroform layer was dried and concentrated and purified on a silica gel column using 4% ethanol in dichloromethane to obtain the product in 50% yield (57 mg).
WORKUP
后处理
- customSolvent was removed under reduced pressure
- customFinally, trifluoroacetic acid was removed under reduced pressure
- customthe crude product was partitioned between chloroform (20 mL) and 7% aqueous NaHCO3 solution (10 mL)
- dry with materialThe chloroform layer was dried
- concentrationconcentrated
- custompurified on a silica gel column
- customto obtain the product in 50% yield (57 mg)