HRID492144

反应详情

EQUATION

反应方程式

HRID 492144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.4 g of 5-difluoromethoxy-2-[[(3,4-dimethoxy-2-pyridinyl)methyl]thio]-1H-benzimidazole was suspended in 6 ml of methanol at room temperature. 0.02 g of Na2WO4·2H2O oxidation catalyst was dissolved in 0.109 g H2O2 (35% aqueous solution), and further diluted with 2 ml of water. The oxidant/catalyst solution was added to the reactant solution dropwise so that the addition was completed in about 30 minutes while stirring at room temperature. The reaction was continued for additional 5.5 hours while stirring. 10 ml of 10% Na2S2O3 aqueous solution was then added, and the resulting mixture was subjected to a reduced pressure to remove methanol therefrom, followed by adding a diluted acetic acid aqueous solution to a pH value of about 8. The resulting pH=8 mixture was extracted with ethyl acetate to obtain a crude product of Pantoprazole with a LC purity of about 52.5%.

WORKUP

后处理

  1. additionThe oxidant/catalyst solution was added to the reactant solution dropwise so that the addition
  2. waitThe reaction was continued for additional 5.5 hours
  3. stirringwhile stirring
  4. customto remove methanol
  5. additionby adding a diluted acetic acid aqueous solution to a pH value of about 8
  6. extractionThe resulting pH=8 mixture was extracted with ethyl acetate