HRID72546
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
- 60 °C
PROCEDURE
实验过程
To a solution of methyl 4-(1-(5-chloro-2-(3-(3-(piperazin-1-yl)phenoxy)azetidin-1-yl)nicotinamido)cyclopropyl)benzoate (D156) (105 mg, 0.186 mmol) in a mixture 1-4-dioxane/water (3 ml/1 ml), 1N NaOH (0.28 ml) was added. The reaction mixture was heated to 60° C. overnight. After cooling at room temperature, the reaction mixture was acidified with 1N HCl (pH=1) and the solvents were evaporated in vacuo. The residue was loaded on Porapak RXN RP cartridge (5 g) eluting with water+0.1% acetic acid/acetonitrile+0.1% acetic acid from 90/10 to 0/100. Collected fractions after solvente evaporation afforded the title compound (E21) (79 mg).
WORKUP
后处理
- temperatureAfter cooling at room temperature
- customthe solvents were evaporated in vacuo
- washeluting with water+0.1% acetic acid/acetonitrile+0.1% acetic acid from 90/10 to 0/100
- customCollected fractions after solvente evaporation