HRID16090
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
PROCEDURE
实验过程
4-bromo-2-chlorobenzoic acid (0.4 g), 5-chloro-2-methoxybenzoic acid (0.4 g), Pd(dppf)Cl2 (0.12 g), sodium carbonate (0.9 g), dioxan (15 ml) and methanol (5 ml) were charged to a flask and heated at reflux for 16 h. Cooled to room temp and filtered (hyflo). The filtrate was concentrated in vacuo, then dissolved in ethyl acetate. The suspension was made basic by addition of dilute NaOH. The aqueous layer was separated and acidified using 2M HCl, extracted with EtOAc, dried (MgSO4) and evaporated in vacuo to give the sub-title compound Yield 0.4 g
WORKUP
后处理
- temperatureheated
- temperatureat reflux for 16 h
- filtrationfiltered (hyflo)
- concentrationThe filtrate was concentrated in vacuo
- dissolutiondissolved in ethyl acetate
- additionThe suspension was made basic by addition of dilute NaOH
- customThe aqueous layer was separated
- extractionextracted with EtOAc
- dry with materialdried (MgSO4)
- customevaporated in vacuo