二新戊基甲酮

反应条件: temp:0.00; pressure:0.00; stir:

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 2,2,6,6-tetramethyl-heptan-4-one (10 g, 0.06 mol), formamidine acetate (33 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 5-tert-butyl-4-(2,2-dimethyl-propyl)-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

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 2,2,6,6-tetramethyl-heptan-4-one (10 g, 0.06 mol), formamidine acetate (33 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 5-tert-butyl-4-(2,2-dimethyl-propyl)-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

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The ratio between dineopentyl ketone and the cyclopropane derivative in this case was 2.26 g/g.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: The ratio between dineopentyl ketone and the cyclopropane derivative in this case was 2.5 g/g.

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 2,2,6,6-tetramethyl-heptan-4-one (10 g, 0.06 mol), formamidine acetate (33 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 5-tert-butyl-4-(2,2-dimethyl-propyl)-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