HRID2258311

反应详情

EQUATION

反应方程式

HRID 2258311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. additionwere added dropwise, at 10° C.
  2. concentrationIt was then concentrated
  3. dissolutionthe residue was dissolved in dichloromethane
  4. additionwere added, at 0° C., to this solution