反应详情

温度

70 °C

A mixture of 2-chloro-5-methyl-pyrimidin-4-ylamine (0.35 g, 2:4 mmol) and 4-(4-amino-benzyl)-piperazine-1-carboxylic acid tert-butyl ester (0.80 g, 2.8 mmol) in acetic acid (20 mL) was heated at 70° C. for 1 d. After cooling to room temperature, the mixture was concentrated. The residue was taken in water (30 mL) and neutralized with 10% NaOH solution until pH˜10. The resulting aqueous layer was extracted with EtOAc (2×30 mL) and the combined organic layers washed with brine, dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated and the title compound used in the next step without purification. MS (ES+): m/z 399 (M+H)+.

1. temperatureAfter cooling to room temperature
2. concentrationthe mixture was concentrated
3. extractionThe resulting aqueous layer was extracted with EtOAc (2×30 mL)
4. washthe combined organic layers washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationThe filtrate was concentrated
8. customthe title compound used in the next step without purification