反应详情

温度

80 °C

To 3.92 g (36.3 mmol, 4 equiv.) of (aminomethyl)cyclopropane hydrochloride was added 2.5 g (44.6 mmol) of potassium hydroxide dissolved in 10 mL of water. The resulting slurry was thoroughly mixed and then dried with 1.0 g of KOH. The free amine was filtered through anhydrous K2CO3 with dry THF rinses (3×2 mL) into 1.44 g (9.08 mmol) of 6-chloro-2,5-dimethyl-4-pyrimidinol. The stirred clear solution was heated at 80° C. for 31/2 days in a sealed 40 mL tube. The cooled, 23° C., mixture was purified by flash chromatography (silica gel, 41 mm column, 5% MeOH in EtoAc as eluant) to afford 1.42 g (7.36 mmol, 81%) of pure product m.p. 227°-228° C.

1. additionThe resulting slurry was thoroughly mixed
2. dry with materialdried with 1.0 g of KOH
3. customThe cooled, 23° C., mixture was purified by flash chromatography (silica gel, 41 mm column, 5% MeOH in EtoAc as eluant)