反应详情

A mixture of 2-(3-bromo-4-methoxyphenyl)ethanamine (1 g; 4.35 mmol), 2-chloro-5-ethyl-pyrimidine (0.56 g; 3.92 mmol) and DIEA (0.84 g; 6.53 mmol) in n-butanol was heated to reflux for 14 hr. Upon cooling, the reaction mixture was concentrated and partitioned between 1N HCl and ether. The aqueous phase was basified with 6N NaOH and extracted with ether. The combined organic phases were washed with a saturated solution of NaHCO3, dried over MgSO4, filtered and concentrated to provide a colorless solid, which was triturated with hexane, filtered and dried to provide the title compound as a white crystalline solid (0.89 g; 67% yield).

1. temperaturewas heated
2. temperatureto reflux for 14 hr
3. temperatureUpon cooling
4. concentrationthe reaction mixture was concentrated
5. custompartitioned between 1N HCl and ether
6. extractionextracted with ether
7. washThe combined organic phases were washed with a saturated solution of NaHCO3
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. concentrationconcentrated
11. customto provide a colorless solid, which
12. customwas triturated with hexane
13. filtrationfiltered
14. customdried