反应 #80291

ord-172b663c480f428491802387607eff65

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The solid was filtered off
  2. 2
    浓缩residue was concentrated under reduced pressure
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The organic layer was washed with water
  5. 5
    干燥dried over anhydrous sodium sulfate
  6. 6
    其他The residue obtained by concentration under reduced pressure
  7. 7
    其他was crystallized from isopropyl ether

实验过程

3.4 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate was dissolved in 50 ml of methanol, and 5 ml of concentrated hydrochloric acid was added thereto. Then, 4.9 g of tin powder was gradually added at room temperature. Them, the mixture was stirred at room temperature for 12 hours. The solid was filtered off, and then residue was concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.5 g (yield: 79%) of the desired product. mp: 132°-135° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05616537uspto-grants-1997_04