HRID627161
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
(2S,5R)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-4-(dimethylcarbamoyl)-5-hydroxy-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 133, 2.194 g, 5.29 mmol) in DCM (65 mL) was cooled in an ice-bath then Dess-Martin periodinane in DCM (26.5 mL, 7.94 mmol) was added and the reaction was stirred at rt overnight. The organic solution was washed with sat. Na2S2O3, sat. NaHCO3, brine, dried over MgSO4, filtered and evaporated. The crude product was purified via flash chromatography (10-75% EA/EtOAc) to obtain the desired product (1.050 g, 48.1%).
WORKUP
后处理
- washThe organic solution was washed with sat. Na2S2O3, sat. NaHCO3, brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
- customThe crude product was purified via flash chromatography (10-75% EA/EtOAc)