反应详情

A mixture of crude {1-[4-(2-bromo-2-phenyl-acetyl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester [Int-1-A] (1.2 g, 82% purity), crude 4-(6-methoxy-pyridin-3-ylmethoxy)-pyrimidin-2-ylamine (0.66 g, 65% purity) and activated 3 Å molecular sieves in EtOH (7.5 mL) was heated at reflux for 2 hours. LC-MS indicated the reaction to be incomplete. A further 0.66 g portion of 4-(6-methoxy-pyridin-3-ylmethoxy)-pyrimidin-2-ylamine was added and the mixture was heated at reflux for 3 hours. On cooling the mixture was partitioned between EtOAc and water, decanted and the separated organic phase washed with brine, dried and concentrated to give the title compound (1.86 g) as a yellow solid which was used in the next step without further purification.

1. temperaturewas heated
2. temperatureat reflux for 2 hours
3. customthe reaction
4. temperaturethe mixture was heated
5. temperatureat reflux for 3 hours
6. temperatureOn cooling the mixture
7. customwas partitioned between EtOAc and water
8. customdecanted
9. washthe separated organic phase washed with brine
10. customdried
11. concentrationconcentrated