反应 #54918

反应方程式

hydroxylamine hydrochloride

water

Hydroxylamine hydrochloride

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

Darco

→

5-Phenyl-2-oxazolecarboxaldehyde Oxime

溶剂

acetic acid

反应条件

后处理

1. 1
   温度was refluxed another five hrs
2. 2
   过滤filtered
3. 3
   workup.ADDITIONpoured into water (5.0 l.)
4. 4
   温度The 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
   温度The solution was cooled
6. 6
   workup.ADDITIONpoured into water (3.0 l.)
7. 7
   其他the resulting solid was collected
8. 8
   其他dried (48 g, 65%)
9. 9
   其他Recrystallization of a sample from acetonitrile
10. 10
    其他gave product of analytical purity, m.p. 208°-210°

实验过程

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°.

来源