반응 #959484

반응 방정식

{1-[4-(2-bromo-2-phenyl-acetyl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester

4-(6-methoxy-pyridin-3-ylmethoxy)-pyrimidin-2-ylamine

4-(6-methoxy-pyridin-3-ylmethoxy)-pyrimidin-2-ylamine

→

title compound

수율 119.2%

(1-{4-[7-(6-methoxy-pyridin-3-ylmethoxy)-3-phenyl-imidazo[1,2-a]pyrimidin-2-yl]-phenyl}-cyclobutyl)-carbamic acid tert-butyl ester

수율 119.2%

용매

EtOH

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 2 hours
3. 3
   기타the reaction
4. 4
   온도the mixture was heated
5. 5
   온도at reflux for 3 hours
6. 6
   온도On cooling the mixture
7. 7
   기타was partitioned between EtOAc and water
8. 8
   기타decanted
9. 9
   세척the separated organic phase washed with brine
10. 10
    기타dried
11. 11
    농축concentrated

실험 절차

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.

출처