HRID1645900

反应详情

EQUATION

反应方程式

HRID 1645900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2.4 g (14.7 mmol) of 3,4-dihydro-5-hydroxy-1(2H)-isoquinolinone and 2.5 g of cesium carbonate in 30 ml of ethanol was added 2.5 g (15.0 mmol) of benzyl bromide. The mixture was stirred for 18 hours at room temperature. Then an additional 2.5 g of cesium carbonate and 2.5 g of benzyl bromide was added and the mixture was heated under reflux conditions for four hours. The reaction was partitioned between water and ether, the ether layer was filtered (to remove solid), dried (MgSO4), and concentrated. The residue was dissolved in hexane, filtered, concentrated, and the residue was crystallized from ethanol to give 3.01 g (81%) of the desired product; mp 171°-173°.

WORKUP

后处理

  1. temperaturethe mixture was heated under reflux conditions for four hours
  2. customThe reaction was partitioned between water and ether
  3. filtrationthe ether layer was filtered
  4. custom(to remove solid)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in hexane
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customthe residue was crystallized from ethanol