반응 #6185

반응 방정식

4-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

propionyl chloride

→

desired compound

수율 74.2%

4-[3-(propionylamino)propylthio]-pyridine

수율 74.2%

용매

methylene chloride

반응 조건

후처리

1. 1
   세척The reaction solution was washed with an aqueous saturated sodium bicarbonate solution and water
2. 2
   기타dried
3. 3
   workup.DISTILLATIONThe solvent was distilled off
4. 4
   기타The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10)
5. 5
   기타to obtain the powder which
6. 6
   세척was washed with ether
7. 7
   기타dried

실험 절차

To a solution of 700 mg (2.90 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 1.62 ml (11.6 mmol) of triethylamine in 30 ml of methylene chloride was added 0.30 ml (3.48 mmol) of propionyl chloride and the mixture was stirred at room temperature for 30 minutes. The reaction solution was washed with an aqueous saturated sodium bicarbonate solution and water and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent: methanol/ethyl acetate=1:10) to obtain the powder which was washed with ether and dried to obtain 483 mg of the desired compound (74.2%, yellow prisms), mp: 50.0°-51.0° C.

출처