反应 #1219480
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07476666B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of ethyl 3-bromo-2-hydroxypropanoate (22.1 g, 112.0 mmol) in EtOH/H2O (1:1) was added sodium azide (10.9 g, 168.0 mmol). The reaction was stirred and heated to 90° C. for 3 days. The EtOH was removed in vacuo and the remaining aqueous solution was extracted with CHCl3 several times. The combined organic extracts were dried over Na2SO4 and concentrated in vacuo to afford the azide as an orange oil. 1H NMR (400 MHz, d6-DMSO) δ 5.96 (d, J=5.6 Hz, 1H), 4.31-4.28 (m, 1H), 4.19-4.08 (m, 2H), 3.51-3.40 (m, 2H), 1.28-1.17 (m, 3H). The EtOH was removed in vacuo the remaining aqueous solution was extracted with CHCl3 several times The combined organic extracts were dried over Na2SO4 concentrated in vacuo
来源 ID: ord-b2e2702fe4a14ab487c9f275c9e007fd