HRID256264

反应详情

EQUATION

反应方程式

HRID 256264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.23 g of 2-amino-4,6-dimethyl pyrimidine in 30 ml of anhydrous acetonitrile was added with stirring 2.7 g of 2-methoxycarbonyl-3-thiophenesulfonylisocyanate. The mixture was heated to the boiling point, whereupon all of the insoluble material dissolved and the mixture was allowed to cool. After stirring for two hours the mixture was filtered to remove the desired product which had precipitated as a white solid. After washing with anhydrous ethyl ether the product melted at 191°-193° with decomposition and showed absorption peaks by nuclear magnetic resonance at 3.8 ppm for the methoxy group, 2.44 ppm for the two methyl groups on the pyrimidine ring, a peak at 7.0 consistent for the hydrogen in the pyrimidine ring and a peak at 7.42 for the hydrogens on the thiophene ring. The infrared absorption spectrum showed absorption peaks at 1720 and 1700 cm-1 consistent for the two carbonyl groups present in the desired product.

WORKUP

后处理

  1. temperatureThe mixture was heated to the boiling point
  2. dissolutionwhereupon all of the insoluble material dissolved
  3. temperatureto cool
  4. filtrationwas filtered
  5. customto remove the desired product which
  6. customhad precipitated as a white solid
  7. washAfter washing with anhydrous ethyl ether the product melted at 191°-193° with decomposition
  8. customabsorption peaks by nuclear magnetic resonance at 3.8 ppm for the methoxy group, 2.44 ppm for the two methyl groups on the pyrimidine ring
  9. customThe infrared absorption spectrum
  10. customabsorption peaks at 1720 and 1700 cm-1 consistent for the two carbonyl groups