HRID1855212

反应详情

EQUATION

反应方程式

HRID 1855212 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a round bottom flask was added methyl 2-(4-(bis(2-chloroethyl)amino)phenyl)acetate (B-4) (3.4 g, 11.68 mmol), LiOH (1.7 g, 70.83 mmol), H2O (100 mL) and THF (50 mL). The reaction mixture was stirred at 50° C. for 2 h. After cooled down to r.t., the reaction mixture was adjusted with HCl (1 N) to pH7 and extracted with EtOAc (100 ml*2), the mixture was dried over Na2SO4 and concentrated under reduced pressure. The crude product (2.8 g) was used next step without further purification. LC-MS: (M+H)+=277;

WORKUP

后处理

  1. temperatureAfter cooled down to r.t.
  2. extractionextracted with EtOAc (100 ml*2)
  3. dry with materialthe mixture was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customwithout further purification