반응 #339537

반응 방정식

1-iodo-3-methoxypropane

4-bromo-1H-pyridin-2-one

→

4-Bromo-2-(3-methoxypropoxy)pyridine

용매

benzene

반응 조건

후처리

1. 1
   온도The mixture is cooled to room temperature
2. 2
   여과filtered through Hyflo
3. 3
   세척The filtercake is washed with benzene and with saturated aqueous sodium hydrogencarbonate solution
4. 4
   기타The phases of the filtrate are separated
5. 5
   추출the aqueous phase is extracted with dichloromethane (3×)
6. 6
   건조The combined organic phases are dried over sodium sulphate
7. 7
   농축concentrated by evaporation

실험 절차

11 mmol of silver carbonate and 20 mmol of 1-iodo-3-methoxypropane [61542-10-7] are added under an argon atmosphere to a solution of 21 mmol of 4-bromo-1H-pyridin-2-one [36953-37-4] in 30 ml of benzene. The reaction mixture is heated to 45° C. with exclusion of light for 2 days. The mixture is cooled to room temperature and filtered through Hyflo. The filtercake is washed with benzene and with saturated aqueous sodium hydrogencarbonate solution. The phases of the filtrate are separated and the aqueous phase is extracted with dichloromethane (3×). The combined organic phases are dried over sodium sulphate and concentrated by evaporation. The title compound is identified on the basis of the Rf value by means of flash chromatography (SiO2 60F).

출처