HRID486985

反应详情

EQUATION

反应方程式

HRID 486985 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution containing 0.34 gram (0.006 mole) of potassium hydroxide and 0.109 gram (0.006 mole) of water in 80 milliliters of ethanol was prepared in a 250 milliliter round bottom flask. With cooling to a temperature of 0° C. in an ice/NaCl bath and stirring, a solution of ethyl 1-(2-methyl-4,5-dichlorophenylaminocarbonyl)cyclopropanecarboxylate prepared in Example III in a small volume of ethanol was added and the mixture allowed to stir with warming to room temperature over a 72 hour period. The mixture was vacuum evaporated to give a white solid residue which was dissolved in water and extracted twice with ether. The ether extracts were discarded. The water solution was acidified to a pH of 2 with 25% HCl solution causing separation of a solid which was taken up into ether, and the acidified aqueous phase was extracted four times. The combined ether extracts were dried over magnesium sulfate and vacuum evaporated to give a white solid. This white solid was water-washed and dried in a vacuum oven to give 1.85 grams (0.006 mole) of 1-(2-methyl-4,5dichlorophenylaminocarbonyl)cyclopropanecarboxylic acid having a melting point of 248° C.-251° C. Elemental analysis of the product indicated the following:

WORKUP

后处理

  1. customwas prepared in a 250 milliliter round bottom flask
  2. stirringto stir
  3. temperaturewith warming to room temperature over a 72 hour period
  4. customevaporated
  5. customto give a white solid residue which
  6. extractionextracted twice with ether
  7. customseparation of a solid which
  8. extractionthe acidified aqueous phase was extracted four times
  9. dry with materialThe combined ether extracts were dried over magnesium sulfate and vacuum
  10. customevaporated
  11. customto give a white solid
  12. washwashed
  13. customdried in a vacuum oven