HRID1985699
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 suspension of 3.5 g of 2-amino-3-cyano-4-benzylamino-6-nitroquinoline in 50 mL of dry pyridine was refluxed with 5.6 g of 4-methoxybenzoyl chloride for 3.5 hours. The solvent was evaporated in reduced pressure and the residue was suspended in 30 mL of a saturated solution of Na2CO3 in water. The suspension was extracted with 3×25 mL of CH2Cl2. The combined organic extract was evaporated to dryness, the residue was dissolved in diethyl ether and the solution was kept in a refrigerator for a night. The precipitate was filtered off, washed with diethyl ether to give 6.25 g of the title compound, m.p.: 145-148° C. LC-MS: MH+ 588; Ret. time: 7.00 min.
WORKUP
后处理
- customThe solvent was evaporated in reduced pressure
- extractionThe suspension was extracted with 3×25 mL of CH2Cl2
- extractionThe combined organic extract
- customwas evaporated to dryness
- dissolutionthe residue was dissolved in diethyl ether
- waitthe solution was kept in a refrigerator for a night
- filtrationThe precipitate was filtered off
- washwashed with diethyl ether