HRID2307538

反应详情

EQUATION

反应方程式

HRID 2307538 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 60 ml of DMF was dissolved 7.62 g (54 mmol) of 1H-1,2,4-triazole-3-carboxylic acid ethyl ester. To the solution were added at room temperature 14 g (108 mmol) of N,N-diisopropylethylamine and 15.8 g (56.7 mmol) of tritylchloride. The mixture was stirred for 2 hours. 300 ml of water and 300 ml of ethylacetate were added thereto. The crystal was filtered, dissolved in 150 ml of chloroform, washed with water and dried. The solvent was removed. The residue was crystallized from ether to give 8.91 g of the titled compound. The ethylacetate layer was washed with water, dried and evaporated. The residue was crystallized from ether to give 4.73 g of the titled compound. 13.64 g of 1-trityl-1,2,4-triazole-3-carboxylic acid ethyl ester was totally obtained. Yield: 66%.

WORKUP

后处理

  1. filtrationThe crystal was filtered
  2. dissolutiondissolved in 150 ml of chloroform
  3. washwashed with water
  4. customdried
  5. customThe solvent was removed
  6. customThe residue was crystallized from ether