反应详情

A mixture of 10 g of 4-methoxy-3,5-dimethylbenzenamine hydrochloride, 19.9 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide, 16.8 g of sodium carbonate, 0.5 g of potassium iodide and 100 ml of cyclohexanol was stirred overnight at 150°-160° C. After cooling, the reaction mixture was poured into water. The product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the solvent was evaporated. The residue was crystallized from 1-butanol, yielding 10 g (50.4%) of 4-(4-methoxy-3,5-dimethylphenyl)-1-[(4-methylphenyl)sulfonyl]piperazine; mp. 174.2° C. (interm. 42).

1. temperatureAfter cooling
2. extractionThe product was extracted with dichloromethane
3. washThe extract was washed with water
4. customdried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column-chromatography over silica gel
8. customThe pure fractions were collected
9. customthe solvent was evaporated
10. customThe residue was crystallized from 1-butanol