تفاعل #6185

معادلة التفاعل

4-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

propionyl chloride

→

desired compound

المردود 74.2%

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

المردود 74.2%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر