HRID464015

反应详情

EQUATION

反应方程式

HRID 464015 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9(R)-bromoacetyl-6,9,11-trihydroxy-5,7,8,9,10,12-hexahydronaphthacene-5,12-dione (1.00 g) obtained in Reference Example 4-(1), sodium valerate (1.44 g) and acetone (50 ml) was stirred under reflux for 2 hours. After removing insoluble matters by filtration, the reaction mixture was concentrated under reduced pressure. The residue was treated with ether (15 ml) and precipitated crystals were collected by filtration to give orange crystals of 9(R)-valeryloxyacetyl-6,9,11-trihydroxy-5,7,8,9,10,12-hexahydronaphthacene-5,12-dione. M.P., 149°-152° C.

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. customAfter removing insoluble matters
  3. filtrationby filtration
  4. concentrationthe reaction mixture was concentrated under reduced pressure
  5. additionThe residue was treated with ether (15 ml)
  6. customprecipitated crystals
  7. filtrationwere collected by filtration