HRID30438
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
A mixture of 0.10 g (0.33 mmol) of N-(4-chloro-phenyl)-8-hydroxy -quinoline-2-carboxamidine, 0.137 g (1 mmol) of K2CO3 and 0.021 g (0.33 mmol) of iodomethane in 3.5 mL of DMF was heated under microwave (100 W, 5 min). It was diluted with 20 mL of NaHCO3, extracted with three 10 mL portions of ether. The combined organic extracts were washed with 10 mL of brine, dried over Na2SO4, filtered and concentrated. The residue was purified by preparative TLC eluting with 20% ethyl acetate in hexanes to give 0.047 g of N-(4-chloro-phenyl)-8-methoxy -quinoline-2-carboxamidine.
WORKUP
后处理
- temperaturewas heated under microwave (100 W, 5 min)
- extractionextracted with three 10 mL portions of ether
- washThe combined organic extracts were washed with 10 mL of brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by preparative TLC
- washeluting with 20% ethyl acetate in hexanes