反应详情

In a mixed solvent of dimethoxyethane (10 ml) and toluene (10 ml) was suspended 1-[(5-chloroindol-2-yl)sulfonyl]-4-[[5-(pyridin-4-yl)pyrimidin-2-yl]carbonyl]piperazine (100 mg) at room temperature, followed by the addition of Lawesson's reagent (2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide, 42 mg). The resulting mixture was heated under reflux for 2 days. After cooling to room temperature, the reaction mixture was concentrated and the residue was purified by chromatography on a silica gel column (3→5% methanol—methylene chloride). 1N hydrochloric acid (in ethanol) was added to make acidic the purified product. After concentration, ethyl acetate was added. Yellow powder so precipitated was collected by filtration and dried, whereby the title compound (34 mg) was obtained.

1. customat room temperature
2. temperatureThe resulting mixture was heated
3. temperatureunder reflux for 2 days
4. concentrationthe reaction mixture was concentrated
5. customthe residue was purified by chromatography on a silica gel column (3→5% methanol—methylene chloride)
6. addition1N hydrochloric acid (in ethanol) was added
7. concentrationAfter concentration, ethyl acetate
8. additionwas added
9. customYellow powder so precipitated
10. filtrationwas collected by filtration
11. customdried