HRID252216

反应详情

EQUATION

反应方程式

HRID 252216 的结构方程式

PROCEDURE

实验过程

The title compound was prepared according to procedures described above, using methyl 2-[(pyridin-3-ylamino)sulfonyl]benzoate and 3-fluorobenzylamine. The title compound was further purified by dissolving 25 g in EtOH (300 mL) and gently heating using water bath to 80° C. The resulting solids material were then slowly dissolved and more EtOH (50 mL) was added to completely dissolve all the solids. The solution left at room temperature to crystallize for 1 h. The resulting crystals were collected and dried under high vacuum for 16 h to afford the title compound as a crystalline solid (21 g, 84%). 1H NMR (400 MHz, DMSO-D6) δ 9.76 (s, 1H) 9.32 (t, 1H) 8.31 (d, 1H) 8.25 (d, 1H) 7.66-7.78 (m, 2H) 7.50-7.65 (m, 3H) 7.39 (q, 1H) 7.23-7.29 (m, 3H) 7.09 (t, 1H) 4.54 (d, 2H).

WORKUP

后处理

  1. customThe title compound was prepared
  2. customThe title compound was further purified
  3. dissolutionby dissolving 25 g in EtOH (300 mL)
  4. temperaturegently heating
  5. customto 80° C
  6. dissolutionThe resulting solids material were then slowly dissolved
  7. additionmore EtOH (50 mL) was added
  8. dissolutionto completely dissolve all the solids
  9. waitThe solution left at room temperature
  10. customto crystallize for 1 h
  11. customThe resulting crystals were collected
  12. customdried under high vacuum for 16 h