反应详情

149 g (1 mole) of 4-tert-butylaniline, 178.5 g (1 mole) of bis-(2-chloroethylamine) hydrochloride and 138 g (1 mole) of potassium carbonate in 600 ml of diethylene glycol dimethyl ether are refluxed for 90 hours. The mixture is rendered strongly alkaline with 1 l of water and concentrated sodium hydroxide solution and stirred for 2 hours. The organic phase is extracted with 3×250 ml of methyl tert-butyl ether and the combined organic phases are washed with 2×250 ml of water, dried over sodium sulfate and evaporated down under reduced pressure. The residue is fractionated under reduced pressure to give 155 g (71% of theory) of a product of boiling point 114°-117° C./0.01 mbar and melting point 48°-52° C.

1. extractionThe organic phase is extracted with 3×250 ml of methyl tert-butyl ether
2. washthe combined organic phases are washed with 2×250 ml of water
3. dry with materialdried over sodium sulfate
4. customevaporated down under reduced pressure
5. customto give 155 g (71% of theory) of a product of boiling point 114°-117° C./0.01 mbar and melting point 48°-52° C.