HRID911777
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
Ethyl 3-(2-(3-benzoylthioureido)-5-bromopyridin-3-yloxy)-4-chlorobenzoate (8.05 g, 15.1 mmol) and K2CO3 (10.4 g, 75.3 mmol) were placed in ethanol (150 mL) and heated to reflux for 2 days and then cooled. The reaction mixture was filtered and the filtrate was concentrated, triturated with water, and dried. The remaining solid was dissolved in CH2Cl2 and purified by silica gel chromatography to give ethyl 3-(5-bromo-2-thioureidopyridin-3-yloxy)-4-chlorobenzoate (1.70 g, 26.2% yield).
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 2 days
- temperaturecooled
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated
- customtriturated with water
- customdried
- dissolutionThe remaining solid was dissolved in CH2Cl2
- custompurified by silica gel chromatography