反应详情

5-Butyl-2-(N-tert-butylaminosulfonyl)thiophene-3-boronic acid (300 mg, 1.27 mmol, see step (b) above), 1-(4-bromobenzyl)-1H-imidazole (606 mg, 1.90 mmol, see Example 1(d) above), toluene (15 mL), ethanol (4 mL), NaOH (1.0 M, 4.0 mL, 5.1 mmol) and Pd(PPh3)4 (43.9 mg, 0.038 mmol) were mixed under N2. The mixture was warmed to reflux for 2 hours, diluted with EtOAc (50 mL), washed with water and brine, and dried over MgSO4. The solvent was removed and the residue was separated by column chromatography using chloroform:methanol (20:1) as eluent. The product was not completely pure but was used in the next step without further purification.

1. temperatureThe mixture was warmed
2. temperatureto reflux for 2 hours
3. washwashed with water and brine
4. dry with materialdried over MgSO4
5. customThe solvent was removed
6. customthe residue was separated by column chromatography
7. customwas used in the next step without further purification