反应详情

A mixture of 1-(4-Chlorobutyl)-1,5,6,7-tetrahydroindol-4-one (600 mg) from step 1 and sodium iodide (438 mg) in acetonitrile (10 mL) was heated at reflux for 6 hours. (3,4-Dichlorophenyl)piperazine (581 mg) and potassium carbonate (367 mg) was then added and reflux continued for 16 h. TLC (ethyl acetate:dichloromethane 1:1) showed complete reaction. The reaction was poured into ice cold water (50 mL) and stirred for 0.5 hours. An oil separated out and was isolated from the mixture. The oil was dissolved with dichloromethane (15 mL), washed with water and brine, then dried with sodium sulfate, filtered and the solvent removed under vacuum to yield the title compound as an oil (970 mg).

1. temperaturewas heated
2. temperatureat reflux for 6 hours
3. temperaturereflux
4. customreaction
5. customAn oil separated out
6. customwas isolated from the mixture
7. washwashed with water and brine
8. dry with materialdried with sodium sulfate
9. filtrationfiltered
10. customthe solvent removed under vacuum