HRID479755
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 8 h
- temperatureAfter cooling
- customthe solid which formed
- filtrationwas collected by filtration
- washwashed with H2O
- customdried in vacuo