反应详情

To a solution of ethyl 3-amino-4-[isobutyl(propyl)amino]benzoate (5 g, 0.0179 mol) in dry DCM (50 mL) was added triethyl amine (7.24 g, 0.0716 mol) at RT. Methane sulphonyl chloride (2.67 g, 0.0233 mol) was added in drops at 0° C. The reaction mixture was stirred at RT for 4 h. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in water, extracted with ethylacetate (2×75 mL), washed with 0.5M HCl, brine, dried over sodium sulphate and evaporated to afford the title compound as a yellow oil (6 g, 93%). 1H NMR (DMSO-d6, 400 MHz) δ 8.45 (s, 1H), 7.86 (s, 1H), 7.65 (m, 1H), 7.28 (m, 1H), 4.28 (m, 2H), 3.09 (s, 3H) 3.01 (m, 2H), 2.86 (m, 2H), 1.68 (m, 1H), 1.42 (m, 2H), 1.28 (m, 3H), 0.80 (m, 9H). LC/MS (Method A): 357.0 (M+H)+. HPLC (Method B) Rt 5.09 min (purity: 94.40%).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. dissolutionThe residue was dissolved in water
3. extractionextracted with ethylacetate (2×75 mL)
4. washwashed with 0.5M HCl, brine
5. dry with materialdried over sodium sulphate
6. customevaporated