反应 #3317094
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US03971647
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A solution of 213 g of dodecylformamide (1.0 mole) in 500 ml of anhydrous benzene is added dropwise at 20°-30° to a suspension of 208 g of phosphorus pentachloride (1.0 mole) in 750 ml of anhydrous benezne. After a further 12 hours of stirring at 30°, the reaction mixture is concentrated in vacuo to dryness. The residue is then dissolved in 100 ml of anhydrous benzene, and 202 g of di-isopropylamine (2.0 moles) added dropwise at 40°-50°. The whole is heated for 2 hours at 50°; water and ice are added, and the mixture rendered alkaline with aqueous sodium hydroxide solution. The organic layer is then separated and concentrated by evaporation. The N1,N 1 -diisopropyl-N2 -dodecyl-formamidine obtained as residue boils at 125°-128°C and 0.03 Torr. the reaction mixture is concentrated in vacuo to dryness The residue is then dissolved in 100 ml of anhydrous benzene The whole is heated for 2 hours at 50° The organic layer is then separated concentrated by evaporation
来源 ID: ord-75dbf75339164729b1bbe151e37d3ef5