HRID1154054

反应详情

EQUATION

反应方程式

HRID 1154054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 g of 2-acetylthiomethyl-hexahydro-3-oxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylic acid were heated at 95° C. for 1.5 hours in 2 M hydrochloric acid. The mixture was cooled, the pH was adjusted to 3 by the addition of disodium hydrogen orthophosphate and the aqueous solution was extracted repeatedly with ethyl acetate. The organic extracts were dried over magnesium sulfate and evaporated. After recrystallization of the residue from acetone, there were obtained 1.1 g of hexahydro-2-mercaptomethyl-3-oxo-1H- pyrazolo[1,2-a]pyridazine-5-carboxylic acid having a melting point of 145.5°-147° C.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. extractionthe aqueous solution was extracted repeatedly with ethyl acetate
  3. dry with materialThe organic extracts were dried over magnesium sulfate
  4. customevaporated
  5. customAfter recrystallization of the residue from acetone