反应详情

温度

90 °C

A vial was charged with (S)-3-bromo-7-iodo-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.520 g, 1.102 mmol), DIPA (0.785 mL, 5.51 mmol), Pd(PPh3)4 (0.127 g, 0.110 mmol), copper(I) iodide (0.021 g, 0.110 mmol), and 3,3-dimethyl-1-butyne (0.203 mL, 1.652 mmol) DMF (3 ml) was added, the vial was sealed under argon, and was heated to 90° C. for 60 minutes. The reaction mixture was diluted with 2-MeTHF then washed with water. The organics were dried over MgSO4 and concentrated. Purification of the crude residue by column chromatography gave (S)-3,7-bis(3,3-dimethylbut-1-ynyl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.180 g, 0.421 mmol) as a white solid. [M+H]+=428.0

1. additionwas added
2. customthe vial was sealed under argon
3. washthen washed with water
4. dry with materialThe organics were dried over MgSO4
5. concentrationconcentrated
6. customPurification of the crude residue by column chromatography