反应详情

5 g of 5-(tetrazol-1-yl)-valeric acid chloride are dissolved in 4.5 ml of absolute methylene chloride and, at 0°, this solution is added dropwise to 35.5 ml of a solution of pyridine and H2S in methylene chloride (30 ml of pyridine and 6 g of H2S in 100 ml of methylene chloride). The mixture is then stirred at 0° under a nitrogen atmosphere for 1 hour. The reaction mixture is taken up in chloroform, and the aqueous phase is acidified to pH 2 with 2N H2SO4 and extracted twice with chloroform. The combined organic phases are washed twice with 25 ml of 10% NaHCO3 solution. The pH is then adjusted to 3 with 2N H2SO4 and the title compound is obtained by repeated extraction with chloroform. It is dried over sodium sulphate and concentrated.

1. extractionextracted twice with chloroform
2. washThe combined organic phases are washed twice with 25 ml of 10% NaHCO3 solution