反应详情

温度

120 °C

130 mg (0.30 mmol) of 2-[1-(4-bromothiazol-2-yl]piperidin-4-ylamino]ethanol from step b, 92 mg (0.29 mmol) of 2-(3,3-dimethylindan-5-yl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane, 92 mg (0.03 mmol) of tetrakis(triphenlyphosphine)palladium(0) and 125 mg (1.18 mmol) of sodium carbonate were weighed out, placed under nitrogen. 2.5 ml of dioxane and 0.5 ml of water were added with stirring. The mixture was degassed, homogenised in an ultrasound bath and heated at 120° C. in the microwave for 30 min, diluted with about 20 ml of EA and 20 ml of water and filtered off. The phases were separated, and the water phase was extracted a further once with EA. The organic phases were combined, dried over sodium sulfate, filtered and evaporated. The oily residue was purified by means of preparative HPLC. The product is in the form of the hydrochloride.

1. customThe mixture was degassed
2. stirringhomogenised in an ultrasound bath
3. additiondiluted with about 20 ml of EA and 20 ml of water
4. filtrationfiltered off
5. customThe phases were separated
6. extractionthe water phase was extracted a further once with EA
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe oily residue was purified by means of preparative HPLC