反应 #3724

ord-cc12e5c031414063a4d8c42a97e5d896

反应条件

温度
5°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the resulting yellow precipitate filtered off
  2. 2
    洗涤washed with water (50 ml)
  3. 3
    workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
  4. 4
    洗涤washed twice with water
  5. 5
    干燥The separated organic layer was then dried (anhydrous sodium sulphate)
  6. 6
    浓缩concentrated
  7. 7
    其他to give a crystalline product, yield 73 g (86%), m.pt 168° C.

实验过程

1,3-Di-n-butylxanthine (73 g, 0.28 mol) was dissolved in acetic acid (120 ml) and then treated with concentrated nitric acid (49 g) at 87° C. After 1 hour, the mixture was cooled to 5° C., the resulting yellow precipitate filtered off and washed with water (50 ml). The yellow crystals were dissolved in dichloromethane and washed twice with water. The separated organic layer was then dried (anhydrous sodium sulphate) and concentrated to give a crystalline product, yield 73 g (86%), m.pt 168° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05734051uspto-grants-1998_03