反应详情

A mixture of 8-[(4-bromophenyl)methyl]-4-hydroxymethyl-2-methyl-5,8-dihydro-6H-pyrido[2,3-d]pyrimidin-7-one (490 mg, 1.35 mmol), 2-[(1-tert-butyl)-1H-tetrazol-5-yl]phenylboronic acid (367 mg, 1.49 mmol) (prepared according to J. W. Ellingboe, et al. U.S. Pat. No. 5,149,699), Na2CO3 (287 mg, 2.71 mmol), tetrakis(triphenylphosphine)palladium(0) (78 mg, 0.07 mmol), EtOH (1 mL), water (2 mL), and toluene (6 mL) was heated under reflux for 23 h. The mixture was diluted with EtOAc, washed with saturated aqueous NaHCO3, brine, dried (MgSO4), and concentrated to give a yellow oil. Purification by flash chromatography (5% MeOH/CH2Cl2) gave 590 mg (90%) of product as an off-white foam. An analytical sample (40 mg) was crystallized from ether/acetone, mp 164°-166° C.

1. customprepared
2. temperatureunder reflux for 23 h
3. washwashed with saturated aqueous NaHCO3, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customto give a yellow oil
7. customPurification by flash chromatography (5% MeOH/CH2Cl2)