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
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
These compounds are preferably prepared as set forth as follows. An ester, preferably the monomethyl ester of isophthalic acid or methyl 5-methyl-1,3-isophthalate is dissolved in a THF/DMF mixture. 1,1′-Carbonyldiimidazole is added at 20-25 degrees C. The diisopropyl amide is added. After 3-24 hr of stirring at 20 degrees C. to the reflux temperature of the solvent, the reaction mixture is partitioned between saturated aqueous ammonium chloride and a water immiscible organic solvent such as ethyl acetate. The aqueous layer is separated and extracted twice more with the organic solvent (ethyl acetate). The solvent removed and the residue thus obtained is basified to yield the isophthalic amide (IIa) in 80% yield.
WORKUP
后处理
- customThese compounds are preferably prepared
- customto the reflux temperature of the solvent, the reaction mixture is partitioned between saturated aqueous ammonium chloride
- customThe aqueous layer is separated
- extractionextracted twice more with the organic solvent (ethyl acetate)
- customThe solvent removed
- customthe residue thus obtained