反应详情

6-Bromohexylbut-3-ynyl ether (DE3513885A1) (525 mg) in DMSO (2 ml) was added to a mixture of sodium bicarbonate (1 g) in DMSO (8 ml) at 150° C. with vigorous stirring and nitrogen bubbling through the solution. The mixture was stirred for 20 min at 150° C. and then allowed to cool to room temperature, diluted with diethyl ether and washed with water. The aqueous layer was extracted with diethyl ether and the combined ether layers were washed with dilute hydrochloric acid, brine, dried (MgSO4) and evaporated to dryness to give the title compound (325 mg): IR 1726 cm−1 MS(TSP+ve) m/z 186 (M+MH4)+.

1. stirringThe mixture was stirred for 20 min at 150° C.
2. washwashed with water
3. extractionThe aqueous layer was extracted with diethyl ether
4. washthe combined ether layers were washed with dilute hydrochloric acid, brine
5. dry with materialdried (MgSO4)
6. customevaporated to dryness