反应详情

温度

50 °C

16 q (100 mmol) of nonane-1,9-diol was dissolved in 150 ml of dimethylformamide and instilled in a suspension of 2.88 g (1.20 mmol) of sodium hydride in 100 ml of DMF. It is stirred for 2 hours at 50° C. It is cooled in an ice bath to 0° C. and 17.1 g (100 mmol) of benzyl bromide is instilled within 3 hours. Then, it is stirred for 5 hours at 60° C. The solution is cooled to room temperature, 1 l of water is added and it is extracted 3 times with 150 ml of ether. The combined organic phases are dried on magnesium sulfate and concentrated by evaporation in a vacuum. The remaining oil is chromatographed on silica gel (mobile solvent: hexane/acetone=15:1).

1. temperatureIt is cooled in an ice bath to 0° C.
2. stirringThen, it is stirred for 5 hours at 60° C
3. temperatureThe solution is cooled to room temperature
4. extractionit is extracted 3 times with 150 ml of ether
5. customThe combined organic phases are dried on magnesium sulfate
6. concentrationconcentrated by evaporation in a vacuum
7. customThe remaining oil is chromatographed on silica gel (mobile solvent: hexane/acetone=15:1)