HRID972011

反应详情

EQUATION

反应方程式

HRID 972011 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The obtained ester (VI-7.5 g.) is dissolved in 75 ml. of ethanol and, under stirring, 3.75 g. of KOH are added. The mixture is stirred for further three hours at ambient temperature and evaporated on a rotation evaporator. The residue is dissolved in 30 ml. of water and extracted with two 10 ml.-portions of chloroform. The aqueous layer is stirred for 15 minutes with 0.8 g. of active carbon and, after the separation of the carbon, it is acidified by means of 5% w./w. HCl. The resinous product is extracted with two 70 ml.-portions of ether and washed with two 50 ml. portions of water. After the drying of the ether extract over Na2SO4, it is evaporated to dryness on a rotation evaporator. Yield: 6.0 g. of a resinous product (84.3% theor.), which is crystallized from acetonitrile.

WORKUP

后处理

  1. customevaporated on a rotation evaporator
  2. dissolutionThe residue is dissolved in 30 ml
  3. extractionof water and extracted with two 10 ml
  4. stirringThe aqueous layer is stirred for 15 minutes with 0.8 g
  5. customof active carbon and, after the separation of the carbon, it
  6. extractionThe resinous product is extracted with two 70 ml
  7. wash-portions of ether and washed with two 50 ml
  8. dry with materialAfter the drying of the ether
  9. extractionextract over Na2SO4, it
  10. customis evaporated to dryness on a rotation evaporator
  11. customof a resinous product (84.3% theor.), which is crystallized from acetonitrile