反应详情

Compound 6 (3.70 g) was dissolved in pyridine (100 mL), and N,N-diethylglycin sodium salt (7.66 g) was added to the solution, followed by stirring at room temperature for 1 hour. Subsequently, p-toluenesulfonyl chloride (9.43 g) was added to the mixture, followed by stirring under reflux for 12 hours. After completion of reaction, the solvent was evaporated under reduced pressure. Chloroform (1,000 mL) was added to the residue, and the mixture was washed with water three times. The pH of the aqueous layer was checked by use of a pH testpaper, and adjusted to 4 to 5 with 1N aqueous hydrochloric acid. The organic layer was dried over sodium sulfate anhydrate, and the solvent was evaporated to dryness. The residue was purified by silica gel column chromatography (CHCl3-Hexane), to thereby yield the target product (yield: 3.62 g, 75%).

1. stirringby stirring
2. temperatureunder reflux for 12 hours
3. customAfter completion of reaction
4. customthe solvent was evaporated under reduced pressure
5. additionChloroform (1,000 mL) was added to the residue
6. washthe mixture was washed with water three times
7. dry with materialThe organic layer was dried over sodium sulfate anhydrate
8. customthe solvent was evaporated to dryness
9. customThe residue was purified by silica gel column chromatography (CHCl3-Hexane)