HRID2258311
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
- 20 °C
PROCEDURE
实验过程
1.7 ml of oxalyl chloride (20 mmol), and also 2 drops of N,N-dimethylformamide, dissolved in tetrahydrofuran, were added dropwise, at 10° C. and while stirring, to 2.1 g (10 mmol) of methyl 5-carboxy-3-methoxypyridine-2-carboxylate in 100 ml of anhydrous tetrahydrofuran and the reaction mixture was stirred at 10° C. for 30 min and at 20° C. for 1 h. It was then concentrated and the residue was dissolved in dichloromethane; 6.8 ml (50 mmol) of triethylamine, and then 1.3 g (1.5 ml, 10 mmol) of 3-butoxypropylamine, dissolved in dichloromethane, were added, at 0° C., to this solution.
WORKUP
后处理
- additionwere added dropwise, at 10° C.
- concentrationIt was then concentrated
- dissolutionthe residue was dissolved in dichloromethane
- additionwere added, at 0° C., to this solution