HRID660896

反应详情

EQUATION

反应方程式

HRID 660896 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.88 g (15.9 mmol) of ethyl[3-(4-chlorophenyl)-4-allyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate from Example 214A are placed in 48 ml methanol and stirred with 5 ml 20% aqueous potassium hydroxide for 2 hrs at room temperature. The solution is concentrated to ca. one half, then diluted with water and extracted with ethyl acetate. The aqueous phase is acidified with ca. 2 ml of conc. hydrochloric acid and extracted twice with 100 ml ethyl acetate each time. The last organic extracts are combined, dried over sodium sulphate, filtered and concentrated in vacuo. After drying in high vacuum, 4.20 g (90% of theory) of the target compound are thus obtained.

WORKUP

后处理

  1. concentrationThe solution is concentrated
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. extractionextracted twice with 100 ml ethyl acetate each time
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customAfter drying in high vacuum, 4.20 g (90% of theory) of the target compound
  9. customare thus obtained