反应详情

A mixture of 28.2 g (0.138 mole) of [(2-chloroethyl)sulfonyl]benzene and 20.0 g (0.139 mole) of 4-(N,N-diethylamino)-1-butanamine in 700 ml of acetonitrile was stirred at room temperature for 16 hr. The solvent was removed in vacuo, and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over magnesium sulfate, and the solvent was removed in vacuo. The residue was dissolved in methanol, a solution of 25.0 g (0.278 mole) of oxalic acid was added and a precipitate was collected to give 47.69 g (68.9%) of title compound, a white crystalline solid, mp 158°-165° C. with decomposition.

1. customThe solvent was removed in vacuo
2. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
3. dry with materialThe methylene chloride solution was dried over magnesium sulfate
4. customthe solvent was removed in vacuo
5. dissolutionThe residue was dissolved in methanol
6. customa precipitate was collected