HRID2246530

反应详情

EQUATION

反应方程式

HRID 2246530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customSolvent was removed under reduced pressure
  2. customFinally, trifluoroacetic acid was removed under reduced pressure
  3. customthe crude product was partitioned between chloroform (20 mL) and 7% aqueous NaHCO3 solution (10 mL)
  4. dry with materialThe chloroform layer was dried
  5. concentrationconcentrated
  6. custompurified on a silica gel column
  7. customto obtain the product in 50% yield (57 mg)