反应 #3703620
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06127343
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of N-(4-bromobenzyl)-N-(pyridin-2-yl)pro-pane-1,3-diamine (1.0 g, 3.123 mmol) in chloroform (40 ml) was added 3-morpholinopropyl isothiocyanate (593 mg, 3.123 mmol) and the reaction mixture was stirred for 20 h at reflux temperature. To the reaction mixture was added 10 drops of 3-morpholinopropyl isothiocyanate and the reaction mixture was stirred for an additional 4 h at reflux temperature. The volatiles were evaporated in vacuo and the residue (2.05 g) was dissolved in ethyl acetate (20 ml) and left over night at room temperature. The precipitate was filtered off and washed with ethyl acetate and dried affording 1.20 g (76%) of the title compound as a solid. at reflux temperature the reaction mixture was stirred for an additional 4 h at reflux temperature The volatiles were evaporated in vacuo the residue (2.05 g) was dissolved in ethyl acetate (20 ml) left over night at room temperature The precipitate was filtered off washed with ethyl acetate dried
来源 ID: ord-3bbdcfb309dd4e2aa7cf5c83d0730c30