HRID2293492
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 2.5N 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): δ8.36 (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