反应详情

A solution of dibenzyl iminodiacetate (9.7 g, 0.031 mol) and triethylamine (4.05 g, 0.04 mol) in 30 ml of carbon tetrachloride was added dropwise to a solution of bromoacetyl bromide (8.88 g, 0.044 mol) in 20 ml of carbon tetrachloride at 0° C. and stirring was continued for 30 min. After addition of water, the organic layer was washed with saturated-NaHCO3 solution and saturated-brine, dried with MgSO4, filtered and concentrated under reduced pressure. The residue was purified by flash column chromatography [silica gel, hexane:EtOAc (3:1)] and yielded 12.66 g (94%) of Compound 1; NMR (CDCl3): δ 3.86 (s,2H), 4.25 (s,2H), 5.15 (s,2H), 5.19 (s,2H), 7.3-7.5 (m, 10H).

1. washthe organic layer was washed with saturated-NaHCO3 solution
2. dry with materialsaturated-brine, dried with MgSO4
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by flash column chromatography [silica gel, hexane:EtOAc (3:1)]