HRID1447153
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringStirring
- waitthe reaction is refrigerated overnight
- filtrationthe precipitated solid is filtered
- washwashed with ether
- dry with materialdried under high vacuum over phosphorus pentoxide