反应详情

6.08 g of 2-(3,4-methylenedioxyphenyl)-m-dithiane-1,1,3,3-tetraoxide (prepared as described in Example 2) are stirred under argon with 25 ml of absolute dimethylformamide and treated with 0.8 of a 55% sodium hydride suspension. The mixture is left to react for 0.5 hour at room temperature and for 1 hours at 40° C. After cooling to room temperature, 4.8 g of N-(3-chloropropyl)-3,4-dimethoxy-N-methyl-phenethylamine (prepared as described in Example 3) are added and the mixture is heated at 100° C for 16 hours. The cooled mixture is then poured on to ice and extracted three times with ethyl acetate. The organic extracts are washed with water, dried over magnesium sulphate and evaporated in vacuo. The residual oil is dissolved in acetone and treated with 5 ml of a 6-N hydrogen chloride solution in dioxane. The precipitate, which is filtered off under a vacuum, is recrystallized from acetone. There are obtained 7.5 g of N-3,4-dimethoxyphenethyl)-N-methyl-2-(3,4-methylenedioxyphenyl)-m-dithiane-2-propylamine-1,1,3,3-tetraoxide hydrochloride of melting point 247°-248° C.

1. waitThe mixture is left
2. customto react for 0.5 hour at room temperature and for 1 hours at 40° C
3. temperaturethe mixture is heated at 100° C for 16 hours
4. additionThe cooled mixture is then poured on to ice
5. extractionextracted three times with ethyl acetate
6. washThe organic extracts are washed with water
7. dry with materialdried over magnesium sulphate
8. customevaporated in vacuo
9. dissolutionThe residual oil is dissolved in acetone
10. additiontreated with 5 ml of a 6-N hydrogen chloride solution in dioxane
11. filtrationThe precipitate, which is filtered off under a vacuum
12. customis recrystallized from acetone