反应详情

To a solution of 4-chloro-6-(methoxymethyl)pyrimidine (768 mg, 4.84 mmole) in dry dioxane (10 mL) was added Cs2CO3 (2.37 g, 7.26 mmole), Xanthphos (84 mg, 0.15 mmole), Pd2(dba)3 (44 mg, 0.05 mmole), and tert-butylcarbamate (681 mg, 5.81 mmole) then the mixture was heated to reflux. After 3 hours, the mixture was cooled to room temperature, diluted with H2O, and extracted with CH2Cl2 (3×). The combined organic layers were dried (MgSO4), filtered, and concentrated. Flash column chromatography (35% EtOAc/hexanes) gave the title compound as a pale yellow solid. 1H-NMR (500 MHz, CDCl3) δ 8.74 (s, 1H), 8.04 (s, 1H), 8.00 (bs, 1H), 4.51 (s, 2H), 3.51 (s, 3H), 1.55 (s, 9H).

1. temperaturethe mixture was heated to reflux
2. extractionextracted with CH2Cl2 (3×)
3. dry with materialThe combined organic layers were dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated