HRID1868472
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 solution of crude tert-butyl 5-(2,4-dichlorophenyl)-2-(hydroxymethyl)-7-methylimidazo[1,2-a]pyrimidine-6-carboxylate (400 mg) in CH2Cl2 (6 mL) was added Dess-Martin periodinane (605 mg, 1.43 mmol). After 2 h, the reaction was concentrated under reduced pressure and diluted with EtOAc. The organic layer was washed with satd aq NaHCO3 and brine prior to drying over MgSO4. Filtration, concentration under reduced pressure and purification by silica gel chromatography afforded tert-butyl 5-(2,4-dichlorophenyl)-2-formyl-7-methylimidazo[1,2-a]pyrimidine-6-carboxylate (90 mg, 41% for the two steps) as a light yellow solid.
WORKUP
后处理
- concentrationthe reaction was concentrated under reduced pressure
- additiondiluted with EtOAc
- washThe organic layer was washed with satd aq NaHCO3 and brine
- dry with materialto drying over MgSO4
- filtrationFiltration, concentration
- customunder reduced pressure and purification by silica gel chromatography