反应详情

In a mixture of 1 ml of methanol and 30 ml of chloroform was dissolved 1.5 g of 2-[2-(methylamino)benzylthio]imidazo[4,5-b]pyridine. To the resulting solution was portionwise added under chilling with ice and aqueous sodium chloride solution to -5° C. 1.08 g of m-chloroperbenzoic acid (purity: 80%) over a period of 20 min., maintaining the temperature of the solution at -5° C.±3° C. The reaction mixture was stirred for additional 15 min. at the same temperature, and to the mixture was added a saturated NaHCO3 solution. The resulting mixture was then stirred. The organic phase was separated and extracted with two portions of 14 ml of 0.1N NaOH. The alkaline extracts were combined and neutralized by NH4Cl, and the deposited oil was extracted with chloroform. The chloroform extract was washed with a saturated aqueous sodium chloride solution, dried over sodium sulfate and placed under reduced pressure to distill of the solvent. The residue was crystallized by addition of acetonitrile to give 2-[2-(methylamino)benzylsulfinyl]imidazo[4,5-b]-pyridine. m.p.: 120° C. (decompn.)

1. additionTo the resulting solution was portionwise added
2. temperaturemaintaining the temperature of the solution at -5° C.±3° C
3. stirringThe resulting mixture was then stirred
4. customThe organic phase was separated
5. extractionextracted with two portions of 14 ml of 0.1N NaOH
6. extractionthe deposited oil was extracted with chloroform
7. extractionThe chloroform extract
8. washwas washed with a saturated aqueous sodium chloride solution
9. dry with materialdried over sodium sulfate
10. distillationto distill of the solvent
11. customThe residue was crystallized by addition of acetonitrile