反应详情

To a solution of tert-butyl 2-aminoethylcarbamate (4.81 g) in dehydrated chloroform (10 ml) were added sodium carbonate (1.06 g) and N-(2-bromoethyl)tritylamine (3.66 g), and the mixture was stirred under reflux for 3 hours. To the reaction mixture were added diethyl ether and hexane, and the solution was washed with water. The mixture was extracted with 5% aqueous citric acid solution, and the aqueous layer was washed with diethyl ether. The aqueous layer was then made alkaline with sodium hydrogencarbonate followed by extraction with diethyl ether. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give tert-butyl 2-{[2-(tritylamino)ethyl]amino}ethylcarbamate (1.86 g) as a viscous oil.

1. temperatureunder reflux for 3 hours
2. washthe solution was washed with water
3. extractionThe mixture was extracted with 5% aqueous citric acid solution
4. washthe aqueous layer was washed with diethyl ether
5. extractionfollowed by extraction with diethyl ether
6. washThe organic layer was washed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo