反应 #1799881
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08278473B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 37.7 g (137 mmol) of ethyl 2,3-dibromo-2-methylpropanoate in 176 ml of THF was added 25 ml of 1,8-diazabicyclo[5.4.0]-7-undecene and refluxed for 2 hours. After cooling to room temperature, to the mixture was added 1N HCl and extracted with tert-butyl methyl ether. The organic layer was washed sequentially with a saturated NaHCO3 solution and a saturated NaCl solution, dried over anhydrous MgSO4, and then concentrated under vacuum to obtain 23.8 g of (E)-ethyl 3-bromo-2-methyl-2-propenoate. refluxed for 2 hours extracted with tert-butyl methyl ether The organic layer was washed sequentially with a saturated NaHCO3 solution a saturated NaCl solution, dried over anhydrous MgSO4 concentrated under vacuum
来源 ID: ord-c71a2ce9fb804d5aa7e4eb3d63156736