HRID1527010

反应详情

EQUATION

反应方程式

HRID 1527010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 1 L round bottomed flask charged with a magnetic stir bar was added crude tert-butyl 4-((S)-1-((S)-1,1-dimethylethylsulfinamido)ethyl)piperidine-1-carboxylate (29 g) was taken up in MeOH (200 mL) before addition of a 4 N solution of HCl in 1,4-dioxane (24.06 ml, 96 mmol). The resulting solution was then stirred at room temperature for 1 h at rt. The methanol was then removed in vacuo to afford viscous oil which was treated with sat'd aqueous NaHCO3 (˜500 mL) and extracted with ethyl acetate (2×500 mL). This organic phase was combined, dried with MgSO4, filtered, and solvent was then removed in vacuo affording the title compound (22 g) which was used without further purification.

WORKUP

后处理

  1. additionTo a 1 L round bottomed flask charged with a magnetic stir bar
  2. customThe methanol was then removed in vacuo
  3. customto afford viscous oil which
  4. extractionextracted with ethyl acetate (2×500 mL)
  5. dry with materialdried with MgSO4
  6. filtrationfiltered
  7. customsolvent was then removed in vacuo