HRID279543

反应详情

EQUATION

反应方程式

HRID 279543 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Sodium hydride (0.72 g of a 60% suspension in mineral oil, 18 mmol) was added to a solution of 4-hydroxymethylpyridine (4 g, 36 mmol) in THF (30 ml) and the mixture heated at reflux for 15 minutes. 7-Fluoro-3,4-dihydroquinazolin-4-one (1 g, 6 mmol), (J. Chem. Soc. section B 1967, 449), was added, the THF was removed by evaporation, and the mixture was heated at 120° C. for 30 minutes. The mixture was allowed to cool, diluted with water (40 ml) and was adjusted to pH8 with concentrated hydrochloric acid. The resulting precipitate was collected by filtration, washed with water, then ether and dried under vacuum to give 7-(4-pyridylmethoxy)-3,4-dihydroquinazolin-4-one (1.12 g, 71%).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 15 minutes
  3. customthe THF was removed by evaporation
  4. temperatureto cool
  5. additiondiluted with water (40 ml)
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. dry with materialether and dried under vacuum