Реакция #54918

Уравнение реакции

hydroxylamine hydrochloride

water

Hydroxylamine hydrochloride

1-[[[5-phenyl-2-oxazolyl]methylene]amino]-2,4-imidazolidinedione

Darco

→

5-Phenyl-2-oxazolecarboxaldehyde Oxime

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   Температураwas refluxed another five hrs
2. 2
   Фильтрацияfiltered
3. 3
   workup.ADDITIONpoured into water (5.0 l.)
4. 4
   ТемператураThe solid was again refluxed in a mixture of hydroxylamine hydrochloride (50 g), acetic anhydride (800 ml) and water (80 ml) for four hrs
5. 5
   ТемператураThe solution was cooled
6. 6
   workup.ADDITIONpoured into water (3.0 l.)
7. 7
   Другоеthe resulting solid was collected
8. 8
   Другоеdried (48 g, 65%)
9. 9
   ДругоеRecrystallization of a sample from acetonitrile
10. 10
    Другоеgave product of analytical purity, m.p. 208°-210°

Методика

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°.

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