HRID361491

反应详情

EQUATION

反应方程式

HRID 361491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-(8-nonenyl)-3,7-dimethylxanthine (810 mg, 2.7 mmol), 4-methylmorpholine-N- oxide (340 mg, 2.9 mmol) and 2.5% oxmium tetroxide in t-butanol (3 drops) in acetone (20 mL) and water (20 mL) was stirred for 24 hours. Saturated aqueous sodium dithionite solution (5 mL) was added. After stirring for 15 minutes, the reaction was extracted with 25% ethanol-dichloromethane (4×50 mL). The combined organic portions were dried over sodium sulfate, and the solvents were evaporated under vacuum. The solid residue was recrystallized (ethanol-chloroform), yielding 490 mg (54%) 1-(8,9-dihydroxynonyl)-3,7-dimethylxanthine (inventive compound no. 1561).

WORKUP

后处理

  1. extractionthe reaction was extracted with 25% ethanol-dichloromethane (4×50 mL)
  2. dry with materialThe combined organic portions were dried over sodium sulfate
  3. customthe solvents were evaporated under vacuum
  4. customThe solid residue was recrystallized (ethanol-chloroform)