HRID2046981
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe solution was refluxed for 30-60 minutes when all the solid
- dissolutionhad dissolved
- customThe excess phosphorus was removed under reduced pressure
- additionThe residue was poured
- waitAfter ten minutes
- extractionthe aqueous solution was extracted with ether
- washThe ether solution was washed with cold water
- dry with materialdried with anhydrous sodium sulfate
- customThe product was obtained
- filtrationafter filtering
- customremoving ether under reduced pressure