反应详情

Acetone (3.2 L) and 2-(5-methyl-1H-tetrazol-1-yl)benzoic acid (228 g) were combined then stirred at ambient temperature for 15 minutes. Potassium carbonate (228 g) was added to the reaction mixture in a single portion. lodoethane (366.9 g) was added dropwise to the reaction mixture producing a slight exotherm. The reaction mixture was heated at reflux for about 4 hours then stirred overnight while cooling to ambient temperature. The precipitated salts were removed by filtration then rinsed with acetone. The combined riltrates were evaporated under vacuum. The residue was dissolved in dichloromethane (1.5 L). The dichloromethane solution was washed with water (1.5 L), dried over magnesium sulfate then concentrated under vacuum to provide 227 g of ethyl-2-(5-methyl-1H-tetrazol-1-yl)benzoate as a white solid m. p. 98-100° C.

1. additionlodoethane (366.9 g) was added dropwise to the reaction mixture
2. customproducing a slight exotherm
3. temperatureThe reaction mixture was heated
4. temperatureat reflux for about 4 hours
5. customThe precipitated salts were removed by filtration
6. washthen rinsed with acetone
7. customThe combined riltrates were evaporated under vacuum
8. dissolutionThe residue was dissolved in dichloromethane (1.5 L)
9. washThe dichloromethane solution was washed with water (1.5 L)
10. dry with materialdried over magnesium sulfate
11. concentrationthen concentrated under vacuum