反应详情

温度

50 °C

To a stirred solution of 6-chloro-3-(2-ethoxy-3,4-dioxo-cyclobut-1-enylamino)-2-hydroxy-N-methoxy-N-methyl-benzenesulfonamide (Intermediate A) (1 g, 2.56 mmol) in THF (20 ml) was added 3-aminopentane (0.596 ml, 5.12 mmol). The reaction mixture was heated at 50° C. overnight. The reaction mixture was concentrated in vacuo and dissolved in EtOAc. The EtOAc solution was washed with 1M HCl(aq) and brine. The EtOAc solution was dried (MgSO4) and concentrated in vacuo. The residue was crystallized from toluene to give a solid; [M+H]+ 432.1. 1H NMR (DMSO) 0.9 (6H, t, 2×CH3), 1.5 (2H, m), 1.6 (2H, m), 3.0 (3H, s, CH3), 3.6 (3H, s, CH3), 3.9 (1H, m), 7.2 (1H, d), 8.1 (1H, d), 8.2 (1H, d). 9.4 (1H, s), 10.1 (1H, s).

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutiondissolved in EtOAc
3. washThe EtOAc solution was washed with 1M HCl(aq) and brine
4. dry with materialThe EtOAc solution was dried (MgSO4)
5. concentrationconcentrated in vacuo
6. customThe residue was crystallized from toluene
7. customto give a solid