反应详情

A mixture of 5-bromopyrimidine (3.96 g), 5-hexynol (2.44 g), dicyclohexylamine (4 g) and acetonitrile (50 ml) was de-oxygenated by bubbline nitrogen through the solution for 10 min. BTPC (150 mg) and copper (I) iodide (25 mg) were added and the mixture was heated to 60°-70° under nitrogen for 1 h, cooled and evaporated in vacuo. Ether (175 ml) was added, the mixture filtered and evaporated in vacuo and the residue purified by FCC. Elution with ether followed by System C (19:1-92:8) gave the title compound as a pale yellow oil (3.79 g), t.l.c. (System C 17:3) Rf 0.55.

1. temperaturethe mixture was heated to 60°-70° under nitrogen for 1 h
2. temperaturecooled
3. customevaporated in vacuo
4. additionEther (175 ml) was added
5. filtrationthe mixture filtered
6. customevaporated in vacuo
7. customthe residue purified by FCC
8. washElution with ether