反应详情

温度

40 °C

Sodium hydride (30 mg, 1.23 mmol) was added to a mixture of 4-chloro-2-methylthio-6-(3-trifluoromethyl-phenyl)-pyrimidine (187 mg, 0.62 mmol) and 1-(2-hydroxyethyl)piperidine (120 μl, 0.92 mmol) in dry THF (6 ml). The mixture was heated at 40° C. for 2 h. After cooling, water and tert-butyl-methyl ether were added. The aqueous layer was extracted twice with tBuOMe. The combined organic layers were dried over MgSO4 and concentrated under reduced pressure. The residue was chromatographed over silica gel (eluent: CH2Cl2 to CH2Cl2/MeOH 95/5) to yield the above titled compound: 190 mg (yield: 78%).

1. temperatureAfter cooling
2. extractionThe aqueous layer was extracted twice with tBuOMe
3. dry with materialThe combined organic layers were dried over MgSO4
4. concentrationconcentrated under reduced pressure
5. customThe residue was chromatographed over silica gel (eluent: CH2Cl2 to CH2Cl2/MeOH 95/5)