反应详情

温度

130 °C

A 100 mL reaction flask is charged with 1-(2,6,6-trimethyl-cyclohex-3-enyl)-ethanone (10 g, 0.06 mol, commercially available at IFF), formamidine acetate (31 g, 0.3 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-(2,6,6-trimethyl-cyclohex-3-enyl)-pyrimidine (˜10 g) is obtained.

1. customA 100 mL reaction flask
2. washThe crude mass is washed once with aqueous sulfuric acid (10%, 100 mL)
3. customButanol is recovered by roto-evaporation
4. customThe crude product is further purified with liquid chromatography (Biotage® system)
5. customcrystallized