HRID1093185
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A suspension of 1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ol (0.76 g, 2.5 mmol) in phosphorus oxychloride (20 mL) was heated a sealed tube with a heat gun until all of the starting material was dissolved. After allowing the mixture to cool to room temperature it was concentrated to dryness under reduced pressure, leaving a pale yellow solid which was then triturated with water and collected by Buchner filtration. The solid was further washed with water and dried under house vacuum to provide 4-chloro-1-isopropyl-6-(4-nitrophenyl)-1H-pyrazolo[3,4-d]pyrimidine (0.90 g, >100%) as a pale yellow solid. MS (ES+): 317.7, 319.8 (M+H)+
WORKUP
后处理
- temperaturewas heated a sealed tube with a heat gun until all of the starting material
- dissolutionwas dissolved
- concentrationwas concentrated to dryness under reduced pressure
- customleaving a pale yellow solid which
- customwas then triturated with water
- filtrationcollected by Buchner filtration
- washThe solid was further washed with water
- customdried under house vacuum