反应 #514358

ord-7dc1113bbd7b4f8d8428fb7d109c1458

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction was filtered through a pad of celite
  2. 2
    洗涤washing with EtOH
  3. 3
    浓缩the filtrate was concentrated in vacuo

实验过程

A solution of 1.5 g (7.42 mmol) of 3-nitrobenzenesulfonamide in 50 ml of EtOH containing 150 mg of 10% palladium on carbon was placed on a Parr hydrogenator under H2 for 1 h. The reaction was filtered through a pad of celite washing with EtOH, and the filtrate was concentrated in vacuo to give 1.28 g (100%) of 3-aminobenzenesulfonamide which was used immediately in the next reaction. The tide compound was prepared as in example 21 from 3-aminobenzenesulfonamide using intermediate C. Recrystallization from MeOH/Et2O provided 1.46 g (67%) of title compound as an off-white solid: mp 240°-242° C.; 1H NMR (D2O, 300 MHz) δ 7.86 (d, 1 H, J=8.1 Hz), 7.75 (s, 1 H), 7.63 (t, 1 H, J=8.1 Hz), 7.51 (d, 1 H, J=8.1 Hz), 2.30 (s, 3 H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE037438E1uspto-grants-2001_11