反应详情

温度

150 °C

2,5-dichlorophenylboronic acid (266 mg, 1.39 mmol), 5-(2-bromothiazol-5-ylmethoxy)-2,2,6,6-tetramethylcyclohex-4-ene-1,3-dione (250 mg, 0.7 mmol), toluene (3 ml), caesium carbonate (310 mg, 0.95 mmol) and [1,3-bis(2,6-diisopropyl)imidazol-2-ylidene](3-chloropyridyl)palladium II dichloride (60 mg, 0.12 mmol) are mixed together in a microwave vial and heated to 150° C. for 30 min under microwave irradiation. The reaction mixture is cooled, filtered, evaporated and purified by flash chromatography on silica gel to give an orange oil. The oil is dissolved in diglyme (3 ml) and 1-butyl-3-methyl imidazolium bis(trifluoromethylsulfonyl)imide (0.1 ml) and heated under microwave irradiation at 210° C. for 30 min. The reaction mixture is cooled to room temperature, the solvent is evaporated under reduced pressure and the residue is purified by flash chromatography on silica gel to give 6-[2-(2,5-dichlorophenyl)-5-methylthiazol-4-yl]-2,2,4,4-tetramethylcyclohexane-1,3,5-trione.

1. temperatureThe reaction mixture is cooled
2. filtrationfiltered
3. customevaporated
4. custompurified by flash chromatography on silica gel
5. customto give an orange oil
6. temperatureThe reaction mixture is cooled to room temperature
7. customthe solvent is evaporated under reduced pressure
8. customthe residue is purified by flash chromatography on silica gel