تفاعل #951205

معادلة التفاعل

water

3-[4-(4-pyridylthio)butyl]quinazoline-2(1H)-thion-4(3H)-one

4-(4-chlorobutylthio)pyridine

→

desired product

المردود 97.1%

1,3-bis[4-(4-pyridylthio)butyl]-quinazoline-2(1H)-thion-4(3H)-one dihydrochloride

المردود 97.1%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   استخلاصthe mixture was extracted with ethyl acetate
3. 3
   أخرىThe extract was dried
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   أخرىThe residue was purified by flash column chromatography (eluent:ethyl acetate/ethanol=25:1 to 10:1)

الإجراء التجريبي

To a solution of 515 mg (1.5 mmol) of 3-[4-(4-pyridylthio)butyl]quinazoline-2(1H)-thion-4(3H)-one and 332 mg (1.65 mmol) of 4-(4-chlorobutylthio)pyridine in 15 ml of dimethylformamide, 0.25 ml (1.65 mmol) of 1,8-diazabicyclo-[5.4.0]-7-undecene was added, and the mixture was stirred at 80° C. for 16 hours. After cooling, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried and the solvent was distilled off. The residue was purified by flash column chromatography (eluent:ethyl acetate/ethanol=25:1 to 10:1) to give 0.694 mg of the desired product (97.1% yield; colorless oil).

المصدر