HRID627158
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
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
- additionwas added
- customthe completion of the reaction
- concentrationThe reaction was concentrated
- additionthe diluted with EtOAc
- filtrationfiltered through a disposal
- filtrationfilter
- concentrationThe filtrate was concentrated
- customthe crude product was purified on silica gel column (0-4% MeOH in DCM)