反应详情

A mixture of 4-(2-chloro-pyrimidin-4-yl)-piperazine-1-carboxylic acid tert-butyl ester (100 mg, 0.33 mmol), 3-chlorobenzylamine (0.65 mL, 5.3 mmol) and potassium carbonate (71 mg, 0.67 mmol) in ethanol (5 mL) was heated at reflux for 7 days. The reaction mixture was cooled to room temperature, poured into H2O (15 mL) and extracted with EtOAc (2×20 mL). The combined organic extracts were washed with H2O (3×15 mL), brine, dried (Na2SO4) and concentrated in vacuo. The residue was purified by preparative TLC (10% MeOH in CH2Cl2) to give a yellow solid. The yellow solid was triturated with MeOH (1 mL) and the solid was collected by filtration to give intermediate (I-3a) as a white solid (48.5 mg).

1. temperaturewas heated
2. temperatureat reflux for 7 days
3. extractionextracted with EtOAc (2×20 mL)
4. washThe combined organic extracts were washed with H2O (3×15 mL), brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe residue was purified by preparative TLC (10% MeOH in CH2Cl2)
8. customto give a yellow solid
9. customThe yellow solid was triturated with MeOH (1 mL)
10. filtrationthe solid was collected by filtration