تفاعل #310849

معادلة التفاعل

caustic soda

2-[(2,6-dichlorophenyl)imino]-imidazolidine

sulfuric acid

potassium persulfate

→

2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   أخرىThe temperature is kept below 50° with a cooling bath
2. 2
   استخلاصis extracted with ether
3. 3
   ترشيحThe residue is filtered off from the solution
4. 4
   workup.ADDITIONa potassium carbonate solution is added to the filtrate up to pH 10.5
5. 5
   أخرىThe product which has precipitated
6. 6
   استخلاصis extracted with ethyl acetate
7. 7
   أخرىrecrystallized twice from acetonitrile, whereupon 2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine of melting point 215°, which
8. 8
   أخرىis obtained

الإجراء التجريبي

2.30 g. of 2-[(2,6-dichlorophenyl)imino]-imidazolidine are dissolved in 10 ml. of concentrated sulfuric acid, and 2.97 g. of potassium persulfate are added in portions at room temperature. The temperature is kept below 50° with a cooling bath. The dark solution is diluted with water and rendered highly alkaline with concentrated caustic soda solution. The unreacted starting material is extracted with ether. The aqueous solution is adjusted to pH 7 with glacial acetic acid and then with sodium bicarbonate. The residue is filtered off from the solution and a potassium carbonate solution is added to the filtrate up to pH 10.5. The product which has precipitated is extracted with ethyl acetate and recrystallized twice from acetonitrile, whereupon 2-[(2,6-dichlorophenyl)imino]-1-hydroxyimidazolidine of melting point 215°, which is identical to the product obtained in Example 3, is obtained.

المصدر