反应详情

4.00 g of 2-amino-5-methylbenzoic acid was dissolved in 40 mL of 1,4-dioxane, to which 5.5 mL of triethylamine and 6.8 mL of diphenylphosphoryl azide were successively added, and this mixture was stirred for 1.5 hours while heating it under reflux. The reaction mixture, to which a mixture of ethyl acetate and water was added, was adjusted to pH 7 with 1M hydrochloric acid, and the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous sodium sulfate, and the solvent was distilled out under reduced pressure to yield 2.96 g of 5-methyl-1,3-dihydro-2H-benzimidazol-2-one as light yellow solid.

1. additionwere successively added
2. temperaturewhile heating it
3. temperatureunder reflux
4. additionwas added
5. customthe organic phase was separated
6. washAfter the resultant organic phase was washed with water
7. dry with materiala saturated sodium chloride solution successively, the washed phase was dried over anhydrous sodium sulfate
8. distillationthe solvent was distilled out under reduced pressure