反应详情

Cyclohexylamine (10 mmol) was added dropwise to 4-chlorobenzylisothio-cyanate (10 mmol) dissolved in 20 ml of dry ether. The solution was stirred for 2 hours at room temperature. The precipitated product was filtered off and crystallized from ethyl acetate. 3-Piperidinopropyl chloride hydrochloride (3 mmol), the product (3 mmol), and ca-talytic amounts of potassium iodide were refluxed in ethanol for 6 days. Sub-sequently, ethanol was evaporated, and the residue was purified by column chromato-graphy (eluent: methylene chloride/methanol (95/5)). After evaporation of the solvent the product was crystallized with hydrochloric acid from diethyl ether/ethanol.

1. filtrationThe precipitated product was filtered off
2. customcrystallized from ethyl acetate
3. customSub-sequently, ethanol was evaporated
4. customthe residue was purified by column chromato-graphy (eluent: methylene chloride/methanol (95/5))
5. customAfter evaporation of the solvent the product
6. customwas crystallized with hydrochloric acid from diethyl ether/ethanol