HRID76146
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
- 45 °C
PROCEDURE
实验过程
To 10.0 g (58.3 mmol) (2-chloropyridyl)-5-acetic acid in 150 mL THF are added 9.45 g (58.3 mmol) CDI and the mixture is stirred at 45° C. for 1 h. Then 28.0 g (291 mmol) NH4CO3 are added and the mixture is stirred at r.t. over night. The reaction mixture is poured onto water and extracted with EtOAc. The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The residue is triturated with TBME and recrystallized from EtOH.
WORKUP
后处理
- stirringthe mixture is stirred at r.t. over night
- additionThe reaction mixture is poured onto water
- extractionextracted with EtOAc
- dry with materialThe organic layer is dried with MgSO4
- customthe solvent is removed in vacuo
- customThe residue is triturated with TBME
- customrecrystallized from EtOH