HRID52893

反应详情

EQUATION

反应方程式

HRID 52893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.65 ml of a 1N aqueous solution of sodium hydroxide were added to a solution of 0.31 g of ethyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate hydrochloride [prepared as described in Example 18(b)] in 6 ml of methanol, and the resulting mixture was allowed to stand overnight at room temperature. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure to remove the methanol. The concentrate was diluted with water and its pH was adjusted to a value of 3 by the addition of dilute hydrochloric acid, after which it was extracted with ethyl acetate. The organic extract was dried over anhydrous sodium sulfate and then concentrated by evaporation under reduced pressure. The resulting residue was triturated with diisopropyl ether, to give 0.15 g of the title compound, melting at 166°-169° C.

WORKUP

后处理

  1. concentrationAt the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure
  2. customto remove the methanol
  3. additionThe concentrate was diluted with water and its pH
  4. additionwas adjusted to a value of 3 by the addition of dilute hydrochloric acid
  5. extractionafter which it was extracted with ethyl acetate
  6. extractionThe organic extract
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. concentrationconcentrated by evaporation under reduced pressure
  9. customThe resulting residue was triturated with diisopropyl ether