HRID2046981

反应详情

EQUATION

反应方程式

HRID 2046981 的结构方程式

PROCEDURE

实验过程

To 40 mL of phosphorus oxychloride and 3 mL. of dimethylaniline is added 2.2 g of crude 4-hydroxy-3-methyl-6-methylmercaptopyrazolo[3,4-d]pyrimidine. The solution was refluxed for 30-60 minutes when all the solid had dissolved. The excess phosphorus was removed under reduced pressure. The residue was poured with vigorous stirring onto a mixture of ice water. After ten minutes, the aqueous solution was extracted with ether. The ether solution was washed with cold water and dried with anhydrous sodium sulfate. The product was obtained after filtering and removing ether under reduced pressure. 215.0 (M+1)+.

WORKUP

后处理

  1. temperatureThe solution was refluxed for 30-60 minutes when all the solid
  2. dissolutionhad dissolved
  3. customThe excess phosphorus was removed under reduced pressure
  4. additionThe residue was poured
  5. waitAfter ten minutes
  6. extractionthe aqueous solution was extracted with ether
  7. washThe ether solution was washed with cold water
  8. dry with materialdried with anhydrous sodium sulfate
  9. customThe product was obtained
  10. filtrationafter filtering
  11. customremoving ether under reduced pressure