تفاعل #6204

معادلة التفاعل

4-(3-aminopropylthio)pyridine dihydrochloride

triethylamine

3,5-dimethoxybenzoyl chloride

→

desired compound

المردود 87.7%

4-[3-(3,5-dimethoxybenzoylamino)propylthio]pyridine

المردود 87.7%

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 995 mg (4.96 mmol) of 3,5-dimethoxybenzoyl 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 1.21 g of the desired compound (87.7%, pale yellow powder), mp: 110.0°-111.0° C.

المصدر