HRID479755

反应详情

EQUATION

反应方程式

HRID 479755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture containing 4-[4-(4-fluorophenyl)-5-(4-pyridyl)-1H-imidazol-2-yl]benzoic acid, sodium salt (0.20 g, 0.5 mmol) [See Ex. 9 above] and concentrated HCl (10 drops) in MeOH (5 mL) was heated at reflux for 8 h. After cooling, the pH was adjusted to neutral by the addition of 2.5 N NaOH, and the solid which formed was collected by filtration, washed with H2O and dried in vacuo. The title compound was obtained as a yellow solid (0.14 g, 76%) and was recrystallized from EtOAc/CH2Cl2; 1H NMR (CDCl3/MeOH-d4); d 8.36 (d, 2H); 8.03 (m, 4H); 7.60 -7.30 (m, 4H); 7.07 (t, 2H); 3.84 (s, 3H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 8 h
  3. temperatureAfter cooling
  4. customthe solid which formed
  5. filtrationwas collected by filtration
  6. washwashed with H2O
  7. customdried in vacuo