反应详情

A suspension of tert-butyl 1-(3-aminophenyl)-2-(tert-butyldimethylsilyloxy)ethyl(2-methoxyethyl)carbamate (0.5 g, 1.95 mmol) and 4-bromobenzenesulfonyl chloride (0.99 g) in chloroform (20 mL) was stirred under nitrogen at room temperature. N,N-Diisopropyl ethyl amine (1 mL) was added and the mixture was stirred for 16 hours at 60° C. The solution was diluted with EtOAc (50 mL), washed with water (2×20 mL), 1 M HCl (20 mL) and brine (20 mL) and dried over Na2SO4. Evaporation of the solvents gave a brown oil which was purified by column chromatography (30% EtOAc in hexane) to give the title compound as a light yellow oil (0.3 g).

1. stirringthe mixture was stirred for 16 hours at 60° C
2. washwashed with water (2×20 mL), 1 M HCl (20 mL) and brine (20 mL)
3. dry with materialdried over Na2SO4
4. customEvaporation of the solvents
5. customgave a brown oil which
6. customwas purified by column chromatography (30% EtOAc in hexane)