反应 #1973959

ord-9f50814b21c14cb2a9f1f8344153ca91

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONWhen the addition
  2. 2
    workup.WAITto stand 30 min
  3. 3
    过滤The mixture was then filtered
  4. 4
    洗涤washed with water
  5. 5
    其他dried

实验过程

Methyl 3,5-di-tert-butyl-2-hydroxybenzoate (28.66 g, 108.4 mmol) was dissolved with stirring in 430 mL glacial acetic acid and the resulting mixture was treated drop wise with fuming nitric acid (90%, 179.26 mL). When the addition was complete, the resulting mixture was stirred for 2.5 h. The reaction mixture was poured into a 2.0 L of crushed ice and allowed to stand 30 min. Afterwards, 1.0 L of water was added and the ice water mixture was allowed to melt. The mixture was then filtered, washed with water and dried to provide the title compound (24.57 g, 89%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08501238B2uspto-grants-2013_08