反应 #3434009
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08557876B2
反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 100 mL reaction flask is charged with 2,5-dimethyl-hexan-3-one (10 g, 0.08 mol), formamidine acetate (40 g, 0.4 mol), and butanol (50 mL). The reaction mixture is heated to 130° C. and stirred for 24 hours. The crude mass is washed once with aqueous sulfuric acid (10%, 100 mL) followed by twice with brine (30 mL). Butanol is recovered by roto-evaporation. The crude product is further purified with liquid chromatography (Biotage® system) and then crystallized. Product 4,5-diisopropyl-pyrimidine (˜5 g) is obtained. A 100 mL reaction flask The crude mass is washed once with aqueous sulfuric acid (10%, 100 mL) Butanol is recovered by roto-evaporation The crude product is further purified with liquid chromatography (Biotage® system) crystallized
来源 ID: ord-4549f547729b4506b330b46577f30bed