반응 #54918

반응 방정식

hydroxylamine hydrochloride

water

Hydroxylamine hydrochloride

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

Darco

→

5-Phenyl-2-oxazolecarboxaldehyde Oxime

용매

acetic acid

반응 조건

후처리

1. 1
   온도was refluxed another five hrs
2. 2
   여과filtered
3. 3
   workup.ADDITIONpoured into water (5.0 l.)
4. 4
   온도The 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
   온도The solution was cooled
6. 6
   workup.ADDITIONpoured into water (3.0 l.)
7. 7
   기타the resulting solid was collected
8. 8
   기타dried (48 g, 65%)
9. 9
   기타Recrystallization of a sample from acetonitrile
10. 10
    기타gave product of analytical purity, m.p. 208°-210°

실험 절차

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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