HRID242897

反应详情

EQUATION

反应方程式

HRID 242897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe volatiles were removed under reduced pressure
  2. customthe residue partitioned between DCM
  3. extractionThe aqueous phase was extracted with DCM (×3)
  4. washthe combined organic fractions washed with water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo