反应详情

2-chloro-4-methanesulfonyl benzoic acid 3.87 g (0.0165 mol) was added to 40 ml of tert.-butanol, and then were added thereto 3.47 g (0.0168 mol) of N,N'-dicyclohexylcarbodiimide and 1.21 g (0.088 mol) of anhydrous potassium carbonate. The resulting mixture was incorporated with 1.65 g (0.0168 mol) of 1-methyl-5-hydroxypyrazole with stirring at room temperature and heated at 60° C. to effect reaction for 5 hours. After completion of the reaction, solvent was distilled away from the reaction mixture under reduced pressure and the resulting residue was washed with chloroform. Thereafter, the residue was incorporated with 30 ml of water and stirred. Insoluble matter was filtered out. The aqueous solution thus obtained was incorporated with conc. hydrochloric acid to adjust the pH thereof to 1 or lower and then with chloroform to effect extraction. An organic layer was separated, dried over anhydrous sodium sulfate, freed of solvent by distillation under reduced pressure, and dried to give 2.75 g of the final product (yield: 53%), m.p. 272°-275° C.

1. additionwere added
2. temperatureheated at 60° C.
3. customreaction for 5 hours
4. customAfter completion of the reaction, solvent
5. distillationwas distilled away from the reaction mixture under reduced pressure
6. washthe resulting residue was washed with chloroform
7. stirringstirred
8. filtrationInsoluble matter was filtered out
9. customThe aqueous solution thus obtained
10. extractionextraction
11. customAn organic layer was separated
12. dry with materialdried over anhydrous sodium sulfate
13. distillationfreed of solvent by distillation under reduced pressure
14. customdried