反应详情

1-(3-chloro-4-(2-cyclopropyl-1-oxoisoindolin-5-yl)benzyl)-3-methylimidazolidine-2,4-dione (0.073 mmol, 30 mg), trimethylboroxine (0.110 mmol, 27.6 mg), tris(dibenzylideneacetone)dipalladium(0) (3.66 μmol, 3.4 mg), tricyclohexylphosphine (8.78 μmol, 2.5 mg) and potassium phosphate, tribasic (0.124 mmol, 26.4 mg) were suspended in dioxane (750 μL) and water (250 μL) and heated under microwave irradiation at 130° C. for 30 minutes. The solvent was removed under reduced pressure and the mixture partitioned between water and dichloromethane. The organic layer was separated using a hydrophobic frit and concentrated. Purified by acidic prep HPLC to afford 1-(4-(2-cyclopropyl-1-oxoisoindolin-5-yl)-3-methylbenzyl)-3-methylimidazolidine-2,4-dione (11.2 mg, 39%); 1H NMR (400 MHz, CDCl3) 7.86 (d, 1H), 7.36 (dd, 1H), 7.31 (d, 1H), 7.21-7.12 (m, 3H), 4.58 (s, 2H), 4.36 (s, 2H), 3.79 (s, 2H), 3.07 (s, 3H), 2.96 (m, 1H), 2.24 (s, 3H), 0.97-0.87 (m, 4H). LCMS (M+H) 390.2.

1. customThe solvent was removed under reduced pressure
2. customthe mixture partitioned between water and dichloromethane
3. customThe organic layer was separated
4. concentrationconcentrated
5. customPurified by acidic prep HPLC