HRID2212111
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
Adapted the alternative method for the preparation of 4d as follows: To the solution of the crude dione 15 (0.413 g, 1.429 mmol) in 50 ml of dry CHCl3 was added N-isopropyl-N′-(ethylcarbonyl)guanidine (0.206 g, 1.191 mmol). The reaction mixture was heated at 50° C. for 48 hours. The reaction was quenched with water, extracted with chloroform and dried over Na2SO4. The solvent was removed in vacuo and the crude product was purified with a silica gel column using 3% EtOAc/CHCl3 as eluent to yield 4a as a white solid (0.115 g, 20%).
WORKUP
后处理
- customThe reaction was quenched with water
- extractionextracted with chloroform
- dry with materialdried over Na2SO4
- customThe solvent was removed in vacuo
- customthe crude product was purified with a silica gel column