HRID1614190

反应详情

EQUATION

反应方程式

HRID 1614190 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The hydroxypyrimidinone of Example 60 (0.2 g, 0.61 mmol) is dissolved in 5 ml ethanol, treated with 2.5 ml 1N NCl and refluxed for 6 hours. The reaction is cooled to room temperature, quenched with water and the product extracted 3× ethyl acetate. The organics are washed, dried, filtered and concentrated in vacuo to yield a crude substance which is crystallized from ethyl acetate to give 60 ml (31.5%) of the pyrimidinone as a crystalline solid. This material is a 7:3 mixture of endo-exo bicycloalkyl isomers.

WORKUP

后处理

  1. additiontreated with 2.5 ml 1N NCl
  2. temperaturerefluxed for 6 hours
  3. customquenched with water
  4. extractionthe product extracted 3× ethyl acetate
  5. washThe organics are washed
  6. customdried
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto yield a crude substance which
  10. customis crystallized from ethyl acetate