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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To trifluoroacetic acid (10 mL), stirred at 0° C., was added tert-butyl mesitylsulfonyloxycarbamate (6.50 g, 20.6 mmol), and the mixture was stirred at 0° C. for 30 min. The mixture was poured into ice-water (10 mL). A white precipitate was formed, which was filtered and collected. The white precipitate was dissolved in DCM (20 mL), and dried with Na2SO4. To the DCM solution was added 1,6-naphthyridin-5-amine (1.0 g, 6.88 mmol), and the mixture was stirred at room temperature for 4 h. The solvent was removed under reduced pressure and the residue was washed with Et2O (3×15 mL). The yellow solid obtained was used in the next step without further purification (3.30 g). ESI MS: m/z 161 [M+H]+.
WORKUP
后处理
- customA white precipitate was formed
- filtrationwhich was filtered
- customcollected
- dissolutionThe white precipitate was dissolved in DCM (20 mL)
- dry with materialdried with Na2SO4
- stirringthe mixture was stirred at room temperature for 4 h
- customThe solvent was removed under reduced pressure
- washthe residue was washed with Et2O (3×15 mL)
- customThe yellow solid obtained
- customwas used in the next step without further purification (3.30 g)