HRID1606522

反应详情

EQUATION

反应方程式

HRID 1606522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.6 g of sodium hydroxide was dissolved in 40 ml of water, and 2.0 g of 5-hydroxycarbostyril and 2.5 g of epichlorohydrin were added to the solution. The mixture was stirred at a temperature of from 60° to 70°C for 5 hours followed by cooling to precipitate the product. The precipitated crystals were washed with water, dissolved in ethanol and then subjected to thin layer chromatography using acetone as an eluate to obtain two spots having a Rf value of 0.58 and 0.65, respectively, The spot having a Rf value of 0.58 was extracted with ethanol and crystallized to obtain 5-(2,3-epoxy)propoxycarbostyril which was used as the starting material in Examples 1 and 2. The spot having a Rf value of 0.65 was worked up in the same manner as described above to obtain 5-(2-hydroxy-3-chloro)propoxycarbostyril which was used as the starting material in Example 3.

WORKUP

后处理

  1. temperatureby cooling
  2. customto precipitate the product
  3. washThe precipitated crystals were washed with water
  4. dissolutiondissolved in ethanol
  5. customto obtain two spots
  6. extractionwas extracted with ethanol
  7. customcrystallized