反应详情

温度

60 °C

A mixture of ethyl 2,7-dichloro-4-(chloromethyl)-6-methoxy-3-quinolinecarboxylate (6.9 g, 20 mmol) and N-methylpiperazine (9 ml, 80 mmol) is heated to 60° C. for 30 min. The reaction mass is diluted with water and extraction is carried out with ethyl acetate. After decanting, the organic phase is washed with water, followed by drying over magnesium sulphate, filtering and evaporating under reduced pressure. The residue is taken up in water, agitated for 15 minutes, filtered, washed with water and dried under vacuum. The residue is purified by column chromatography (SiO2, MeOH/CH2Cl2: 5/95 to 8/92). 6.7 g of product, a beige solid, is obtained.

1. customAfter decanting
2. washthe organic phase is washed with water
3. dry with materialby drying over magnesium sulphate
4. filtrationfiltering
5. customevaporating under reduced pressure
6. filtrationfiltered
7. washwashed with water
8. customdried under vacuum
9. customThe residue is purified by column chromatography (SiO2, MeOH/CH2Cl2: 5/95 to 8/92)