反应详情

温度

0 °C

4-(1-furan-2-yl-ethyl)-morpholine (1.1 mmol) was taken up in DCM (5 ml) and stirred at 0° C. Nitrogen was passed through the reaction vessel and bubbled out through a Dreschel bottle containing a saturated aqueous solution of sodium thiosulphate, whilst bromine (1.54 mmol in 2 ml DCM) was added dropwise. After addition the reaction was stirred at room temperature for 2 h, then diluted with more DCM, washed twice with 2M Na2CO3 solution, dried over Na2SO4 and concentrated in-vacuo. After purification by flash chromatography (silica, 5 to 10% EtOAc in hexane), 4-[1-(5-bromo-furan-2-yl)-ethyl]-morpholine was obtained as a golden oil: m/z in MS ES+=260, 262 [M+H]+, 0.46 mmol, 42% yield.

1. custombubbled out through a Dreschel bottle
2. additionwas added dropwise
3. additionAfter addition the reaction
4. stirringwas stirred at room temperature for 2 h
5. washwashed twice with 2M Na2CO3 solution
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in-vacuo
8. customAfter purification by flash chromatography (silica, 5 to 10% EtOAc in hexane)