HRID2420698

反应详情

EQUATION

反应方程式

HRID 2420698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pyrrolidine (3.0 mL; 35.9 mmol) was added to glycolic acid (2.73 g; 35.9 mmol) over 5 minutes while cooling in an ice bath. The suspension was diluted with o-xylene (3.5 mL) and heated to reflux for 7 h whereupon the o-xylene was removed by distillation to afford the title compound (4.17 g; 90%) as an orange oil. 1H NMR (CDCl3) δ 1.86-4.92 (m, 2H), 1.96-2.02 (m, 2H), 3.26-3.29 (m, 2H), 3.52-3.55 (m, 3H), 4.08 (s, 2H); 13C NMR (CDCl3) δ 23.94, 25.74, 44.26, 45.96, 60.48, 169.90.

WORKUP

后处理

  1. temperaturewhile cooling in an ice bath
  2. temperatureheated
  3. customwas removed by distillation