反应详情

0.6 g (2.46 mmol) 4,6-dichloro-3-nitro-quinoline (Example 23c) and 0.247 ml (2.71 mmol) aniline in 4 ml acetic acid are stirred at rt for 4 h (tlc-control). A precipitate is formed. The reaction mixture is poured into 150 ml water. The solid is filtered off and washed with water and hexane. The filtrate is dissolved in ca. 50 ml diethylether, filtered from insoluble material, and the solvent is evaporated. The residue, yellow crystals, is dried at 60° C. over night. mp: 174-175° C. MS: 300 (M++1); HPLC: tret=10.53 min (Grad 1).

1. customA precipitate is formed
2. filtrationThe solid is filtered off
3. washwashed with water and hexane
4. dissolutionThe filtrate is dissolved in ca. 50 ml diethylether
5. filtrationfiltered from insoluble material
6. customthe solvent is evaporated
7. customThe residue, yellow crystals, is dried at 60° C. over night
8. customtret=10.53 min (Grad 1)