HRID1399600

反应详情

EQUATION

反应方程式

HRID 1399600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl 2-(4-methyl-2-(4-methylpiperazin-1-yl)-6-p-tolylpyrimidin-5-yl)pentanoate (0.042 g; 0.105 mmol) in methanol (2 mL) was added a solution of sodium hydroxide 5N (0.131 mL; 0.656 mmol) and the reaction mixture was heated to reflux for 48 h. The volatiles were removed under reduced pressure, the residue dissolved in water and the pH was adjusted to 5 by addition of a solution of hydrochloric acid 2N. The formed precipitate was collected by filtration and dried under reduced pressure. Purification by preparative HPLC (HPLC method 4) furnished 0.043 g (58%) of the title compound as a solid.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 48 h
  3. customThe volatiles were removed under reduced pressure
  4. dissolutionthe residue dissolved in water
  5. additionthe pH was adjusted to 5 by addition of a solution of hydrochloric acid 2N
  6. filtrationThe formed precipitate was collected by filtration
  7. customdried under reduced pressure
  8. customPurification by preparative HPLC (HPLC method 4)