反应详情

0.100 g (0.29 mmol) of 6-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]-2-methyl-4H-3,1-benzoxazin-4-one in 2 ml of a 20% aqueous ammonia solution are heated for 2 hours at 50° C. and then hydrolysed with 3 ml of 10% aqueous sodium hydroxide solution and brought to 50° C. for 2 hours. The reaction medium is acidified with a 1N aqueous solution of hydrochloric acid, to pH=9. The precipitate obtained is filtered off, rinsed with water and then dried under reduced pressure at 40° C. overnight. The solid obtained is purified by silica gel column chromatography, elution being carried out with a dichloromethane/methanol (90/10) mixture. 67 mg of a yellow solid are obtained.

1. customThe precipitate obtained
2. filtrationis filtered off
3. washrinsed with water
4. customdried under reduced pressure at 40° C. overnight
5. customThe solid obtained
6. customis purified by silica gel column chromatography, elution