反应详情

To a suspension of 2-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (D69) (3 g), 2-bromo-1,3-thiazole (1.659 g) and Cs2CO3 (3.95 g) in 1,2-dimethoxyethane (DME) (40 mL)/water (10 mL) stirred under nitrogen at room temperature was added PdCl2(dppf)-CH2Cl2 adduct (661 mg) in one charge. The reaction vessel was sealed and heated under microwave at 120° C. for 2 h. After cooling the reaction, the reaction mixture was filtered and the filtrate was partitioned between ethyl acetate (150 mL) and saturated brine (50 mL). The organic phase was dried over sodium sulphate and evaporated in vacuo. The crude product was purified by column chromatography to give 2-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,3-thiazole (D70) (1.5 g). MS (ES): C12H12ClNOS requires 253. found 254.1 (M+H+).

1. additioncharge
2. customThe reaction vessel was sealed
3. temperatureheated under microwave at 120° C. for 2 h
4. temperatureAfter cooling
5. customthe reaction
6. filtrationthe reaction mixture was filtered
7. customthe filtrate was partitioned between ethyl acetate (150 mL) and saturated brine (50 mL)
8. dry with materialThe organic phase was dried over sodium sulphate
9. customevaporated in vacuo
10. customThe crude product was purified by column chromatography