反应详情

To a solution of bromoacetyl bromide (30 g) in methylene chloride (20 ml) at 0° was added a solution of N-methyl-4-nitrobenzenemethanamine (8.3 g; G. I. Wilson, J. Chem. Soc., 1926, 2461) in methylene chloride (10 ml) and triethylamine (12 ml). The reaction was stirred 5 min. at 0° and then water (20 ml) was added. The methylene chloride layer was dried and evaporated in vacuo. The residue was purified by column chromatography eluting with methylene chloride/methanol (97:3) to give the title compound (15 g) as an oil. NMR includes signals at d 3.1(3H,s,N--CH3); 3.9(2H,s,CH2Br); 4.55(2H,s,Ph--CH2 --N); 7.0-8.3(4H,m,aromatics).

1. dry with materialThe methylene chloride layer was dried
2. customevaporated in vacuo
3. customThe residue was purified by column chromatography
4. washeluting with methylene chloride/methanol (97:3)