反应详情

0.96 g (0.02 mol) of 50% sodium hydride dispersion are freed from the mineral oil with absolute tetrahydrofuran and suspended in 30 cc of tetrahydrofuran. A solution of 1.56 g (0.02 mol) of 2-mercaptoethanol in 10 cc of tetrahydrofuran is added at 20°-25° while stirring, to this suspension. The mixture is stirred at 60° over the course of 10 hours. After this period a solution of 4.3 g (0.02 mol) of piperonyl bromide in 30 cc of tetrahydrofuran is added dropwise to the mixture. The reaction mixture is stirred at 60° over the course of 8 hours, subsequently cooled to 20° and 100 cc amounts of ether and water are added. The organic phase is separated off in a separating funnel, extracted with saturated sodium chloride solution, dried over sodium sulphate and evaporated. The residue may be purified by chromatography on silica gel with hexane/ethyl acetate (1:2). 2-Piperonylthio-ethanol is obtained as a colourless oil, which according to gas-chromatography is pure.

1. stirringThe mixture is stirred at 60° over the course of 10 hours
2. stirringThe reaction mixture is stirred at 60° over the course of 8 hours
3. temperaturesubsequently cooled to 20°
4. customThe organic phase is separated off in a separating funnel
5. extractionextracted with saturated sodium chloride solution
6. dry with materialdried over sodium sulphate
7. customevaporated
8. customThe residue may be purified by chromatography on silica gel with hexane/ethyl acetate (1:2)