반응 #361907

반응 방정식

water

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

4-(4-chlorobutylthio)pyridine

1,8-diazabicyclo[5.4.0]-7-undecene

→

desired product

수율 97.1%

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

수율 97.1%

용매

dimethylformamide

반응 조건

후처리

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

실험 절차

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).

출처