تفاعل #928237

معادلة التفاعل

3-(2-phenylthiothiazol-5-yl-methyl)-5-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine

hydrochloric acid

chlorine

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title product

3-(2-Chloro-thiazol-5-yl-methyl)-5-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine

المذيبات

chlorobenzene

ظروف التفاعل

المعالجة

1. 1
   أخرىexcess chlorine is removed by the introduction of nitrogen
2. 2
   أخرىthe phases are then separated
3. 3
   ترشيحfiltered
4. 4
   غسيلthe filtration residue is washed with water
5. 5
   أخرىdried in vacuo at 50° C

الإجراء التجريبي

183 g of 3-(2-phenylthiothiazol-5-yl-methyl)-5-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine are introduced over a period of 5 minutes, with stirring, into a mixture of 300 g of hydrochloric acid (32%) and 150 g of chlorobenzene. 124 g of chlorine are introduced at 20° C. over a period of 4 hours. After 2 hours, excess chlorine is removed by the introduction of nitrogen, and the phases are then separated. The aqueous phase is adjusted to pH 5 with sodium hydroxide solution (30%) and then filtered, and the filtration residue is washed with water and dried in vacuo at 50° C. The title product is obtained in a purity of 97%.

المصدر