反应详情

温度

100 °C

(4-Trimethylstannyl-thiazol-2-ylmethyl)-carbamic acid tert-butyl ester (191 mg, 0.507 mmol) and [3-Methyl-4-(6-methyl-pyridin-3-yloxy)-phenyl]-(6-iodo-quinazolin-4-yl)-amine hydrochloride (0.251 g, 0.478 mmol) (from Step C, Example 3) are dissolved in anhydrous DMF under a nitrogen atmosphere. Hunig's base (0.44 ml, 2.53 mmol), and PdCl2(PPh3)2 are added to the reaction mixture at room temperature. The reaction mixture is degassed and heated at 100° C. overnight. After cooling to room temperature the reaction mixture is diluted with water and thoroughly extracted with EtOAc and DCM. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure. Flash chromatography on silica with EtOAc-MeOH as an eluant affords 81 mg (0.14 mmol, 28%) of clean desired product.

1. customThe reaction mixture is degassed
2. temperatureAfter cooling to room temperature the reaction mixture
3. additionis diluted with water
4. extractionthoroughly extracted with EtOAc and DCM
5. dry with materialThe combined organic extracts are dried (Na2SO4)
6. concentrationconcentrated under reduced pressure