反应详情

A mixture of 84.2 g of 4-methanesulphonyl-2,2-dimethyl-1-nitrosopiperazine, 90.5 g of thiourea dioxide, 200 ml of ethanol and 200 ml of water is cautiously treated with 85 g of caustic soda and heated to reflux for 30 hours. After cooling, the mixture is filtered and the product is isolated from the filtrate by extraction with methylene chloride. After drying over sodium sulphate and concentrating the methylene chloride solution, the oil which remains is dissolved in a little ethanol and precipitated as the hydrochloride by addition of ethanolic hydrochloric acid.

1. temperatureheated
2. temperatureto reflux for 30 hours
3. temperatureAfter cooling
4. filtrationthe mixture is filtered
5. customthe product is isolated from the filtrate by extraction with methylene chloride
6. dry with materialAfter drying over sodium sulphate
7. concentrationconcentrating the methylene chloride solution
8. dissolutionthe oil which remains is dissolved in a little ethanol
9. customprecipitated as the hydrochloride by addition of ethanolic hydrochloric acid