反应详情

温度

120 °C

A mixture of compound 2,4-dichloro-6-phenyl-pyrimidine (0.5 g, 2.22 mmol), 4-aminocyclohexanol hydrochloride (0.12 g, 1.11 mmol), triethylamine (0.67 g, 6.62 mmol) in n-butanol (10 mL) was stirred at 120° C. for 12 hours under a nitrogen atmosphere. The reaction mixture was then concentrated under vacuum, diluted with water (25 mL) and extracted with ethyl acetate (3×20 mL). The organic layers were collected, combined, washed with water (20 mL), dried over anhydrous sodium sulphate, and concentrated under vacuum. The residue thus obtained was purified by column chromatography using ethyl acetate-petroleum ether to give the two compounds 4-(2-chloro-6-phenyl-pyrimidin-4-ylamino)-cyclohexanol and 4-(4-chloro-6-phenyl-pyrimidin-2-ylamino)-cyclohexanol in ratio 1:2 (overall yield: 63%).

1. concentrationThe reaction mixture was then concentrated under vacuum
2. additiondiluted with water (25 mL)
3. extractionextracted with ethyl acetate (3×20 mL)
4. customThe organic layers were collected
5. washwashed with water (20 mL)
6. dry with materialdried over anhydrous sodium sulphate
7. concentrationconcentrated under vacuum
8. customThe residue thus obtained
9. customwas purified by column chromatography