反应详情

温度

50 °C

A mixture of 5-bromo-6-(2-phenylethynyl)pyridin-2-amine B2a (20 g, 73 mmol), (3,5-dimethyl-1,2-oxazol-4-yl)boronic acid (24 g, 170 mmol), CsF (44 g, 289 mmol) tris-(dibenzylideneacetone)dipalladium(0) (10.28 g, 11.2 mmol), tri-tert-butylphosphonium tetrafluoroborate (8.6 g, 296 mmol) and THF (200 ml) is stirred under argon atmosphere at 50° C. for 1 h. The mixture is filtrated and the precipitate washed with THF. The combined organic layers are concentrated in vacuo, diluted with DCM and extracted with a saturated aqueous solution of NaHCO3. The combined organic layers are dried over MgSO4 and concentrated in vacuo. The product is purified by NP chromatography. Yield: 12.2 g (58%). HPLC-MS: M+H=290; tR=1.54 min (*Method—6).

1. filtrationThe mixture is filtrated
2. washthe precipitate washed with THF
3. concentrationThe combined organic layers are concentrated in vacuo
4. additiondiluted with DCM
5. extractionextracted with a saturated aqueous solution of NaHCO3
6. dry with materialThe combined organic layers are dried over MgSO4
7. concentrationconcentrated in vacuo
8. customThe product is purified by NP chromatography