反应 #7593

ord-aeca40a5c11b49e09fe5ba429ff41801

溶剂

反应条件

温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取After extraction with ethyl acetate
  2. 2
    洗涤the organic layer was washed with water
  3. 3
    干燥brine, dried (MgSO4)
  4. 4
    其他the solvent evaporated
  5. 5
    过滤The solid was filtered off
  6. 6
    洗涤washed with hexane
  7. 7
    其他dried under vacuum

实验过程

The starting material 5-benzyloxy-2-fluoro-4-methylnitrobenzene was obtained by adding benzyl bromide (3 ml, 25 mmol) to a solution of 2-fluoro-5-hydroxy-4-methylnitrobenzene (3.92 mg, 23 mmol) in DMF (70 ml) containing potassium carbonate (9.5 g, 68 mmol). After stirring for 3 hours at 60° C. the mixture was diluted with water and adjusted to pH2. After extraction with ethyl acetate, the organic layer was washed with water and then brine, dried (MgSO4) and the solvent evaporated. The solid was filtered off, washed with hexane and dried under vacuum to give 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.83 g, 80%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07087602B2uspto-grants-2006_08