反应详情

温度

150 °C

A mixture of (S)-tert-butyl 2-(4-bromophenyl)morpholine-4-carboxylate (100 mg, 0.29 mmol), 1-(4-fluorophenyl)-1H-pyrazole-4-ylboronic acid (60 mg, 0.29 mmol), tribasic potassium phosphate (124 mg, 0.585 mmol) and tetrakis(triphenylphosphine)palladium(0) (13.5 mg, 0.0117 mmol) in dimethylacetamide (2 ml) was placed in a microwave tube, closed and heated at 150° C. for 10 min using a microwave synthesizer (Personal Chemistry Emrys Optimizer). After cooling water (10 ml) was added, and the reaction mixture was extracted with ethyl acetate. The aqueous phase was re-extracted with ethyl acetate twice. The combined organic layers were dried (MgSO4) and evaporated. The residue was purified by flash chromatography (12 g silica gel, 10 to 50% ethyl acetate in heptane) to yield a light brown solid (45 mg, 36%). MS (ISP): 424.1 ([M+H]+).

1. customwas placed in a microwave tube
2. customclosed
3. additionwas added
4. extractionthe reaction mixture was extracted with ethyl acetate
5. extractionThe aqueous phase was re-extracted with ethyl acetate twice
6. dry with materialThe combined organic layers were dried (MgSO4)
7. customevaporated
8. customThe residue was purified by flash chromatography (12 g silica gel, 10 to 50% ethyl acetate in heptane)