反应详情

To a mixture of 300 g of aqueous hydrochloric acid (32%) and 150 g of chlorobenzene are added with stirring 186 g of 3-(2-cyclohexylthiothiazol-5-ylmethyl)-5-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine within 5 minutes. 124 g of chlorine are then passed into the mixture at 20 to 25° over a period of 4 hours. After stirring for a further 2 hours, the excess of chlorine is removed by introduction of nitrogen, and the aqueous phase (containing the title compound in hydrochloride form) is separated off and adjusted to pH 5 with aqueous sodium hydroxide solution (30%). The crystalline precipitate is filtered off, washed with water and dried at 50° in vacuo, yielding 135 g of the title compound (purity: 97%) melting at 132 to 135°.

1. additionare added
2. customthe excess of chlorine is removed by introduction of nitrogen
3. additionthe aqueous phase (containing the title compound in hydrochloride form)
4. customis separated off
5. filtrationThe crystalline precipitate is filtered off
6. washwashed with water
7. customdried at 50° in vacuo