HRID627158

反应详情

EQUATION

反应方程式

HRID 627158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of N-(allyloxy)-N-((3R,6S)-6-((tert-butyldimethylsilyloxy)methyl)-1,2,3,6-tetrahydropyridin-3-yl)-2,4-dinitrobenzenesulfonamide (Intermediate 127, 17.50 g, 33.10 mmol) and potassium carbonate (13.73 g, 99.31 mmol) in acetonitrile (700 mL), benzenethiol (5.10 ml, 49.65 mmol) was added. The reaction mixture was stirred at rt for 2.5 hours. LCMS showed the completion of the reaction. The reaction was concentrated, the diluted with EtOAc and filtered through a disposal filter. The filtrate was concentrated and the crude product was purified on silica gel column (0-4% MeOH in DCM) to get the desired product as a yellow oil (5.6 g).

WORKUP

后处理

  1. additionwas added
  2. customthe completion of the reaction
  3. concentrationThe reaction was concentrated
  4. additionthe diluted with EtOAc
  5. filtrationfiltered through a disposal
  6. filtrationfilter
  7. concentrationThe filtrate was concentrated
  8. customthe crude product was purified on silica gel column (0-4% MeOH in DCM)