反应详情

温度

60 °C

To a solution of methyl 2,4-dichloro-3-(4,5-dihydro-4-methyl-5-oxo-1H-tetrazol-1-yl)benzoate (4.10 g) in dioxane (70 ml), 10N sodium hydroxide (2.0 ml) and water (4ml) were added and the mixture was stirred at 60° C. for 1.5 hours. After concentrating under reduced pressure and the addition of water (50 ml), an aqueous solution of sodium hydroxide was added and washed with ethyl acetate (150 ml). The aqueous layer was acidified with hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with saturated salt water and dried with anhydrous magnesium sulfate. By distilling off of ethyl acetate, the objective 2,4-dichloro-3-(4,5-dihydro-4-methyl-5-oxo-1H-tetrazol-1-yl)benzoic acid (3.42 g, yield 87%) was obtained. mp: 221-225° C.

1. concentrationAfter concentrating under reduced pressure
2. additionthe addition of water (50 ml)
3. additionan aqueous solution of sodium hydroxide was added
4. washwashed with ethyl acetate (150 ml)
5. extractionextracted with ethyl acetate
6. washThe organic layer was washed with saturated salt water
7. dry with materialdried with anhydrous magnesium sulfate
8. distillationBy distilling off of ethyl acetate