反应详情

0.251 g (0.83 mmol) of triphosgene diluted in 3 ml of dioxane is added, under an inert atmosphere at ambient temperature, to 0.4 g (1.18 mmol) of methyl 2-amino-5-[(1-methoxy-2-methylindolizin-3-yl)carbonyl]benzoate in 10 ml of dioxane. After stirring for 2.5 hours, 0.267 g (2.36 mmol) of O-prop-2-en-1-ylhydroxylamine and 0.82 ml (5.91 mmol) of triethylamine are added. The reaction medium is stirred for one hour and then hydrolysed with water. The aqueous phase is extracted with dichloromethane. The organic phase obtained is washed with a 1N aqueous solution of hydrochloric acid and a saturated aqueous solution of sodium chloride, and then dried over sodium sulphate, filtered, and concentrated under reduced pressure. 0.581 g of a yellow solid is obtained.

1. stirringThe reaction medium is stirred for one hour
2. extractionThe aqueous phase is extracted with dichloromethane
3. customThe organic phase obtained
4. washis washed with a 1N aqueous solution of hydrochloric acid
5. dry with materiala saturated aqueous solution of sodium chloride, and then dried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure