反应详情

To a solution of 2-mercaptoindole (1.34 g, 8.98 mmol) and 2-chloromethyl-5-methyl-4-piperidinopyridine hydrochloride (2.35 g, 9.00 mmol) in ethanol (90 ml) was added a 2N aqueous sodium hydroxide solution (9.0 ml) under ice-cooling, and the mixture was stirred at room temperature for 30 minutes. After the removal of the organic solvent by evaporation under a reduced pressure, a saturated sodium chloride solution was added to the residue and the mixture was extracted with chloroform. The chloroform layer separated was dried over anhydrous magnesium sulfate and then concentrated in vacuo. The residue was purified by a silica gel column chromatography [eluent: chloroform and then chloroform-methanol (50:1)] whereby to yield the titled compound (2.51 g) as a crystalline substance.

1. temperaturecooling
2. customAfter the removal of the organic solvent
3. customby evaporation under a reduced pressure
4. additiona saturated sodium chloride solution was added to the residue
5. extractionthe mixture was extracted with chloroform
6. customThe chloroform layer separated
7. dry with materialwas dried over anhydrous magnesium sulfate
8. concentrationconcentrated in vacuo
9. customThe residue was purified by a silica gel column chromatography [eluent