HRID1985699

反应详情

EQUATION

反应方程式

HRID 1985699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solvent was evaporated in reduced pressure
  2. extractionThe suspension was extracted with 3×25 mL of CH2Cl2
  3. extractionThe combined organic extract
  4. customwas evaporated to dryness
  5. dissolutionthe residue was dissolved in diethyl ether
  6. waitthe solution was kept in a refrigerator for a night
  7. filtrationThe precipitate was filtered off
  8. washwashed with diethyl ether