HRID1252601

反应详情

EQUATION

反应方程式

HRID 1252601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 2-(hydroxymethyl)-5-(phenylmethoxy)-4(1H)-pyridinone (3 g, 12.99 mmole) in chloroform (15 ml) was cooled to 0° under argon and treated with thionyl chloride (6.1 ml, 83.62 mmole). Within several minutes, a homogeneous solution was obtained. After stirring an additional 5 minutes, a cream colored solid precipitated. The cooling bath was removed and the mixture was heated at reflux for 45 minutes. The mixture was cooled to 0° and the white precipitate was filtered, washed with chloroform and hexane and dried in vacuo. The yield of the title compound was 3.65 g.

WORKUP

后处理

  1. temperaturewas cooled to 0° under argon
  2. waitWithin several minutes
  3. customa homogeneous solution was obtained
  4. customprecipitated
  5. customThe cooling bath was removed
  6. temperaturethe mixture was heated
  7. temperatureat reflux for 45 minutes
  8. temperatureThe mixture was cooled to 0°
  9. filtrationthe white precipitate was filtered
  10. washwashed with chloroform and hexane
  11. customdried in vacuo