HRID530959

反应详情

EQUATION

反应方程式

HRID 530959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
92.5 °C

PROCEDURE

实验过程

In a clean round bottom flask, 10 gm of 1-[(4-Methylquinazolin-2yl)methyl]-3-methyl-7-(2-butin-1yl)-8-(3(R)-4-methylphthalimidopiperidine-yl) xanthine and 100 ml of toluene were charged. 10 ml of ethanolamine was added to the reaction mass and heated to 90-95° C. to complete the reaction. The reaction mass was cooled to 80° C. and the layers were separated. The organic phase was distilled under vacuum to get crude linagliptin. Dry wt: 7.50 gm HPLC purity: 97.95% Impurity X: 0.69%

WORKUP

后处理

  1. customthe reaction
  2. temperatureThe reaction mass was cooled to 80° C.
  3. customthe layers were separated
  4. distillationThe organic phase was distilled under vacuum