反应详情

4.0 g (17 mmol) 6-hydroxy-7-methoxy-4-(1-methylethyl)-2H-1-benzopyran-2-one (example 105), 4.7 g (20.5 mmol) 1-(3-chloropropyl)-4-phenylpiperazine, 4.7 g (34 mmol) potassium carbonate and 1.0 g potassium iodide are agitated in 300 ml DMF for 44 h under nitrogen at 60° C. After filtration and removal of the solvent in vacuum, the residue is taken up in chloroform and washed with dilute sodium hydroxide solution and with water, dried over sodium sulfate and then evaporated again. Yield 5.5 g (74%) of crystals with a fusion point of 94°-96° C. (from isopropanol and TBME). Fumarate: method E; yield 88%; fusion point 175°-176° C. (from isopropanol and ethanol).

1. filtrationAfter filtration and removal of the solvent in vacuum
2. washwashed with dilute sodium hydroxide solution and with water
3. dry with materialdried over sodium sulfate
4. customevaporated again
5. customwith a fusion point of 94°-96° C. (from isopropanol and TBME)
6. customfusion point 175°-176° C. (from isopropanol and ethanol)