HRID1886010

反应详情

EQUATION

反应方程式

HRID 1886010 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-bromopyrimidine (3.96 g), 5-hexynol (2.44 g), dicyclohexylamine (4 g) and acetonitrile (50 ml) was de-oxygenated by bubbling 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.

WORKUP

后处理

  1. customby bubbling nitrogen through the solution for 10 min
  2. additionBTPC (150 mg) and copper (I) iodide (25 mg) were added
  3. temperaturethe mixture was heated to 60°-70° under nitrogen for 1 h
  4. temperaturecooled
  5. customevaporated in vacuo
  6. additionEther (175 ml) was added
  7. filtrationthe mixture filtered
  8. customevaporated in vacuo
  9. customthe residue purified by FCC
  10. washElution with ether