HRID552195

反应详情

EQUATION

反应方程式

HRID 552195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of commercially available itaconic acid and N,N-dimethylethylenediamine was heated up to 160° C. for about 20-25 minutes. The mixture was allowed to cool to 100° C. and then diluted with MeOH to prevent solidification. The product was obtained in a 56% yield after crystallization from MeOH/EtOAc. 1H-NMR (300 MHz, D2O): δ 2.63 (dd, 1H), 2.80 (dd, 1H), 2.95 (s, 6H), 3.15-3.25 (m, 1H), 3.32-3.44 (m, 1H), 3.44-3.76 (m, 4H), 3.82-3.94 (m, 1H). Retention Time (LC, method: ammonium acetate standard): 0.13 min. MS (M+H+): 201.0.

WORKUP

后处理

  1. temperatureto cool to 100° C.
  2. customThe product was obtained in a 56% yield
  3. customafter crystallization from MeOH/EtOAc
  4. custom0.13 min