反应详情

The product of step (i) (3.00 g) and N-bromosuccinimide (2.02 g) in carbon tetrachloride (50 ml) was heated at reflux temperature for 64 hours. The solvent was evaporated and the black residue dissolved in methanol/ethyl acetate, treated with charcoal, filtered and then evaporated. The resulting brown oil was purified by flash chromatography on silica, eluting with dichloromethane. Trituration with hexane gave methyl N-[4-(bromoacetyl)phenoxyacetyl]glycinate, 0.85 g, as a solid: mp softens 109°-111° C.; NMR (d6DMSO) δ 8.60 (1H, bt), 7.99 (2H, d), 7.09 (2H, d), 4.84 (2H, s), 4.69 (2H, s), 3.91 (2H, d), 3.64 (3H, s).

1. temperatureat reflux temperature for 64 hours
2. customThe solvent was evaporated
3. dissolutionthe black residue dissolved in methanol/ethyl acetate
4. additiontreated with charcoal
5. filtrationfiltered
6. customevaporated
7. customThe resulting brown oil was purified by flash chromatography on silica
8. washeluting with dichloromethane