HRID1447153

反应详情

EQUATION

反应方程式

HRID 1447153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4.6 g (15.2 mmol) of the above pyrimidine acid and 25 ml of N,N-dimethylacetamide is stirred at 0°-5° and 4.9 g (30 mmol) of carbonyldiimidazole is added. The mixture is stirred for 2 hrs as the ice bath melts and another 2.5 g (15 mmol) of carbonyldiimidazole is added. Stirring is continued for 2 hrs and 50 ml of tetrahydrofuran is added and the reaction is refrigerated overnight. A 200 ml portion of ether is added and the precipitated solid is filtered, washed with ether, and dried under high vacuum over phosphorus pentoxide to give 5.9 g of 2-[4-(N-ethylcarbamoylamino)phenyl]-4-hydroxy-5-pyrimidine carboxylic acid imidazolide.

WORKUP

后处理

  1. stirringStirring
  2. waitthe reaction is refrigerated overnight
  3. filtrationthe precipitated solid is filtered
  4. washwashed with ether
  5. dry with materialdried under high vacuum over phosphorus pentoxide