反应详情

0.4 g of 80% sodium hydride is added over 5 minutes to a stirred solution, under an argon atmosphere, of 0.6 g of 10-methyl-5H,10H-imidazo-[1,2-a]indeno[1,2-e]pyrazin-4-one in 30 ml of dimethylformamide. The stirring is continued for 10 minutes at a temperature in the region of 20° C., then 0.35 ml of trimethylchlorosilane is added and the stirring is continued for 10 minutes. 82 mg of sodium hydride are then added and the stirring is continued for 1 hour. 0.5 g of 2-chloromethyl-1-methylimidazole hydrochloride is then added and the stirring is continued for 2 hours. The reaction mixture is treated with 6 ml of acetic acid and 200 ml of water. The solution obtained is washed with ethyl acetate (2×200 ml) and the aqueous phase is concentrated on a rotary evaporator. The evaporation residue is triturated with 20 ml of isopropanol and filtered, and the filtrate is concentrated on a rotary evaporator. A pasty residue is obtained which is purified by chromatography on a column of silica (80 g), eluting with a dichloromethane/methanol mixture (85/15 by volume). 0.28 g of 10-methyl-10-[(l-methylimidazol-2-yl)methyl]-5H,10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-4-one is obtained in the form of a cream-coloured solid melting above 260° C. (Analysis, % calculated C: 68.87, H: 5.17, N: 21.13, O: 4.83, % found C: 68.8, H: 5.2, N: 21.2).

1. waitthe stirring is continued for 10 minutes
2. waitthe stirring is continued for 1 hour
3. waitthe stirring is continued for 2 hours
4. customThe solution obtained
5. washis washed with ethyl acetate (2×200 ml)
6. concentrationthe aqueous phase is concentrated on a rotary evaporator
7. customThe evaporation residue is triturated with 20 ml of isopropanol
8. filtrationfiltered
9. concentrationthe filtrate is concentrated on a rotary evaporator
10. customA pasty residue is obtained which
11. customis purified by chromatography on a column of silica (80 g)
12. washeluting with a dichloromethane/methanol mixture (85/15 by volume)