HRID1855212
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooled down to r.t.
- extractionextracted with EtOAc (100 ml*2)
- dry with materialthe mixture was dried over Na2SO4
- concentrationconcentrated under reduced pressure
- customwithout further purification