HRID242897
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 [(S)-1-(2-phenylaminopyridin-3-ylcarbamoyl)propyl]carbamic acid tert-butyl ester (4.32 mmol) in AcOH (30 mL) was heated at 70° C. for 3 h. After cooling to RT, the volatiles were removed under reduced pressure and the residue partitioned between DCM and a saturated aqueous solution of NaHCO3. The aqueous phase was extracted with DCM (×3) and the combined organic fractions washed with water, dried (Na2SO4) and concentrated in vacuo to afford the title compound as an oil (1.27 g, crude material). LCMS (Method C): RT 3.24 min [M+H]+ 353.4.
WORKUP
后处理
- customthe volatiles were removed under reduced pressure
- customthe residue partitioned between DCM
- extractionThe aqueous phase was extracted with DCM (×3)
- washthe combined organic fractions washed with water
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo