HRID1030800

反应详情

EQUATION

反应方程式

HRID 1030800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 20 ml of chloroform was dissolved 900 mg of 2-[2-(isobutylamino)benzylthio]imidazo[4,5-b]pyridine. To the resulting solution was portionwise added under chilling with ice 618 mg of m-chloroperbenzoic acid (purity: 80%) over a period of 30 min. To the mixture was added a saturated NaHCO3 solution, and the resulting mixture was then stirred. The organic phase was separated and extracted successively with 20 ml of 0.1N NaOH and 10 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 off the solvent. The residue was crystallized by addition of diethyl ether. The crystalline product was washed with diethyl ether to give 195 mg of 2-[2-(isobutylamino)benzylsulfinyl]imidazo[4,5-b]pyridine as a pale yellow crystalline powder. m.p.: 116° C. (decompn.)

WORKUP

后处理

  1. additionTo the resulting solution was portionwise added
  2. customThe organic phase was separated
  3. extractionextracted successively with 20 ml of 0.1N NaOH and 10 ml of 0.1N NaOH
  4. extractionthe deposited oil was extracted with chloroform
  5. extractionThe chloroform extract
  6. washwas washed with a saturated aqueous sodium chloride solution
  7. dry with materialdried over sodium sulfate
  8. distillationto distill off the solvent
  9. customThe residue was crystallized by addition of diethyl ether
  10. washThe crystalline product was washed with diethyl ether