反应详情

Hydroxylamine hydrochloride (54 g, 0.78 mole) and 1-[[[5-phenyl-2-oxazolyl]methylene]amino]-2,4-imidazolidinedione (105 g, 0.39 mole) were refluxed with stirring in a solution of water (100 ml) and glacial acetic acid (1.0 l.) for five hrs. An additional 54 g of hydroxylamine hydrochloride was added while the mixture was refluxed another five hrs. The hot solution was treated with Darco, filtered and poured into water (5.0 l.). The solid was again refluxed in a mixture of hydroxylamine hydrochloride (50 g), acetic anhydride (800 ml) and water (80 ml) for four hrs. The solution was cooled, poured into water (3.0 l.) and the resulting solid was collected and dried (48 g, 65%). Recrystallization of a sample from acetonitrile gave product of analytical purity, m.p. 208°-210°.

1. temperaturewas refluxed another five hrs
2. filtrationfiltered
3. additionpoured into water (5.0 l.)
4. temperatureThe solid was again refluxed in a mixture of hydroxylamine hydrochloride (50 g), acetic anhydride (800 ml) and water (80 ml) for four hrs
5. temperatureThe solution was cooled
6. additionpoured into water (3.0 l.)
7. customthe resulting solid was collected
8. customdried (48 g, 65%)
9. customRecrystallization of a sample from acetonitrile
10. customgave product of analytical purity, m.p. 208°-210°