反应详情

温度

60 °C

To a solution of 2.5 g of 2-hydroxy-3',4'-dichlorobibenzyl in 10 ml of dimethylformamide was added 0.23 g of sodium hydride under cooling. The mixture was stirred for 30 minutes and to this was added dropwise 2.2 g of 3-dimethylaminopropyl chloride. The reaction mixture was warmed to about 60° C. and then stirred for 5 hours. Upon completion of the reaction, 2N-NaOH aqueous solution was added, and the product was extracted with ether. The ether extract was washed well with saturated sodium chloride solution, dried over anhydrous sodium sulfate and then distilled in vacuo to sufficiently remove ether and a small amount of the remaining 3-dimethylaminopropyl chloride. The resultant residue was dissolved in ether and then 20% ethanolic hydrogen chloride was added to yield a precipitate. Recrystallization from ethanol-ether gave 2.6 g (71% yield) of 2-(3-dimethylaminopropoxy)-3',4'-dichlorobibenzyl hydrochloride, m. p. 136°-137° C.

1. temperatureunder cooling
2. stirringstirred for 5 hours
3. additionwas added
4. extractionthe product was extracted with ether
5. extractionThe ether extract
6. washwas washed well with saturated sodium chloride solution
7. dry with materialdried over anhydrous sodium sulfate
8. distillationdistilled in vacuo to sufficiently remove ether
9. dissolutionThe resultant residue was dissolved in ether
10. addition20% ethanolic hydrogen chloride was added
11. customto yield a precipitate
12. customRecrystallization from ethanol-ether