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 2 h at 25° C. After addition of water, the organic layer was washed with a 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:EtAOc (3:1)] and yielded 12.66 g (94%) of compound 2. NMR (CDCl3): 3.86 (s,2H), 4.25 (s,2H), 4.27 (s,2H), 5.15 (s,2H), 5.19 (s,2H), 7.3-7.5 (m,10H). Anal. calcd. for C20H20BrNO5 : C, 55.31; H, 4.64; Br, 18.40; N, 3.23. Found: C, 55.38; H, 4.69; Br, 18.46; N, 3.19.

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