HRID1107893

反应详情

EQUATION

反应方程式

HRID 1107893 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-naphthyl carboxylic acid (2.0 g, 11.6 mmol) and N,N'-carbonyldimidazole (2.07 g, 12.8 mmol) in dry tetrahydrofuran (50 ml) was stirred at reflux temperature for 1 h. To the cooled reaction mixture was added 3,5-diamino-1,2,4-triazole (1.15 g, 11.6 mmol) and the resulting mixture was refluxed for 3 h. The cooled reaction mixture was quenched with water (75 ml) and extracted with diethyl ether (2×75 ml). The combined organic extracts were washed with saturated aqueous sodium chloride (2×50 ml), dried (MgSO4), filtered and evaporated in vacuo. The residue was crystallised from diethyl ether (20 ml), filtered off and washed with diethyl ether (2×10 ml), dried in vacuo afforded 0.95 g (32%) of the title compound as a solid.

WORKUP

后处理

  1. temperatureat reflux temperature for 1 h
  2. customTo the cooled reaction mixture
  3. temperaturethe resulting mixture was refluxed for 3 h
  4. customThe cooled reaction mixture
  5. customwas quenched with water (75 ml)
  6. extractionextracted with diethyl ether (2×75 ml)
  7. washThe combined organic extracts were washed with saturated aqueous sodium chloride (2×50 ml)
  8. dry with materialdried (MgSO4)
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe residue was crystallised from diethyl ether (20 ml)
  12. filtrationfiltered off
  13. washwashed with diethyl ether (2×10 ml)
  14. customdried in vacuo