HRID1993844

反应详情

EQUATION

反应方程式

HRID 1993844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The crude product from step (b) above (1.2 g, 3.83 mmol), 1-(4-bromobenzyl)-1H-imidazole (98.8 mg, 0.416 mmol, see Example 1(d) above), Pd(PPh3)4 (29 mg, 0.25 mmol), NaOH (3 mL, 1M, 3 mmol), toluene (15 mL) and ethanol (3 mL) were mixed under N2 (g). The mixture was heated to reflux for 2 h. The reaction mixture was then diluted with ethyl acetate (150 mL) and washed with water and brine. The organic phase was dried over MgSO4 and the solvent was removed in vacuo. Purification using column chromatography with CHCl3: MeOH (20:1) as eluent yielded the sub-title compound (93.7 mg, 0.220 mmol) in 53% yield.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2 h
  3. washwashed with water and brine
  4. dry with materialThe organic phase was dried over MgSO4
  5. customthe solvent was removed in vacuo
  6. customPurification