反应详情

A mixture of N1-(5-bromobenzo[d]isothiazol-3-yl)propane-1,3-diamine (100 mg, 0.35 mmol), phenylboronic acid (43 mg, 0.35 mmol), tetrabutylammonium bromide (115 mg, 0.35 mmol), sodium carbonate (110 mg, 1.05 mmol) and palladium (II) acetate (1 mg) in water (3 mL) was microwaved at 150° C. for 5 min. The reaction was diluted with methylene chloride and the mixture was washed successively with aqueous sodium bicarbonate and brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting product, N1-(5-Phenylbenzo[d]isothiazol-3-yl)propane-1,3-diamine, was carried forward without further purification. MW=238 confirmed by LC-MS, tr=2.73 min (Method B) MH+=237-239

1. customwas microwaved at 150° C. for 5 min
2. washthe mixture was washed successively with aqueous sodium bicarbonate and brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe resulting product, N1-(5-Phenylbenzo[d]isothiazol-3-yl)propane-1,3-diamine, was carried forward without further purification
7. customconfirmed by LC-MS, tr=2.73 min (Method B) MH+=237-239