تفاعل #6203

معادلة التفاعل

4-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

4-t-butylbenzoyl chloride

→

desired compound

المردود 88.0%

4-[3-(4-t-butylbenzoylamino)propylthio]pyridine hydrochloride

المردود 88.0%

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooling
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
3. 3
   غسيلThe reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and water
4. 4
   أخرىdried
5. 5
   workup.DISTILLATIONThe solvent was distilled off
6. 6
   أخرىThe residue was purified by column chromatography (eluent: ethyl acetate)

الإجراء التجريبي

To a solution of 1.00 g (4.15 mmol) of 4-(3-aminopropylthio)pyridine dihydrochloride and 2.77 ml (19.8 mmol) of triethylamine in 40 ml of methylene chloride was added 0.48 ml (4.96 mmol) of 4-t-butylbenzoyl chloride under ice-cooling with stirring and the mixture was stirred at room temperature for 30 minutes. The reaction mixture 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: ethyl acetate) to obtain 1.20 g of the desired compound (free base) (88.0%, yellow powder).

المصدر