反应详情

温度

140 °C

A suspension of 4-bromo-N-(2,4-dimethylphenyl)-N-isobutylbenzenesulfonamide (200 mg, 0.505 mmol), potassium trans-3-bromo-1-propenyltrifluoroborate (126 mg, 0.555 mmol), morpholine (0.088 mL, 1.009 mmol), bis(triphenylphosphine)palladium(II) chloride (10.63 mg, 0.015 mmol) and cesium carbonate (493 mg, 1.514 mmol) was prepared in dimethyl sulfoxide (DMSO) (1 mL). The reaction was then heated by microwaves, to 140° C. for 30 minutes. The reaction was then passed through a sulfonic acid (SCX) solid phase extraction (SPE) cartridge, eluting with methanol followed by ammonia in methanol, then concentrated under a stream of nitrogen. Purification was carried out by mass directed autoprep (ammonium carbonate modifier). The relevant fractions were concentrated and combined to give the desired product, 23.2 mg. LCMS [LCMS2] Rt 1.41 min, m/z (ES+) 443 (M+H).

1. extractionThe reaction was then passed through a sulfonic acid (SCX) solid phase extraction (SPE) cartridge
2. washeluting with methanol
3. concentrationconcentrated under a stream of nitrogen
4. customPurification
5. concentrationThe relevant fractions were concentrated