HRID219991

反应详情

EQUATION

反应方程式

HRID 219991 的结构方程式

PROCEDURE

实验过程

The title compound was obtained following procedure and work up described for example 107, step 1, but starting from 3-(aminosulfonyl)-N′-hydroxybenzenecarboximidamide, prepared as described in WO 2006/013104 A1 from 3-cyanobenzene-1-sulfonamide (Maybridge; GK 03054), (1.50 g; 6.97 mmol) and Intermediate 28 (1.79 g; 6.97 mmol), followed by a recrystallization from DCM gave the title compound as a white powder. 1H NMR (DMSO-d6, 300 MHz) δ 8.58-8.57 (m, 1H), 8.35-8.32 (m, 2H), 8.20-8.17 (m, 1H), 8.08-8.05 (m, 1H), 7.83 (t, J=7.8 Hz, 1H), 7.59 (bs, 2H), 7.43 (d, J=8 Hz, 1H), 7.36-7.27 (m, 3H), 7.16-7.13 (m, 1H), 4.23 (d, J=12.6 Hz, 1H), 4.16 (d, J=12.6 Hz, 1H), 3.25 (s, 3H), 2.03 (s, 3H). LC/MS (Method B): 436.3 (M+H)+. HPLC (Method A) Rt 5.37 min (purity: 99.6%).

WORKUP

后处理

  1. customprepared
  2. customfollowed by a recrystallization from DCM