反应 #2329

ord-045379b86e3a4189977f9bacd7189198

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他the solvent was evaporated in vacuo
  2. 2
    其他to give an orange oil
  3. 3
    过滤A solution of this oil, in a small volume of dichloromethane, was filtered through silica
  4. 4
    其他the clear filtrate, on evaporation

实验过程

Bromine (2.09 ml) was added dropwise over ten minutes to a stirred solution of the product of step (i) above (9.44 g) in carbon tetrachloride (200 ml). The solution was stirred for 16 hours, then the solvent was evaporated in vacuo to give an orange oil. A solution of this oil, in a small volume of dichloromethane, was filtered through silica and the clear filtrate, on evaporation, gave methyl 4-(2-bromo-2,2-dimethylacetyl)phenoxyacetate, 11.3 g, as a white crystalline solid: m.p. 46°-50° C.; NMR (d6DMSO) δ 8.09 (2H, d), 7.05 (2H, d), 4.92 (2H, s), 3.72 (3H, s), 2.0(6H, s).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05728701uspto-grants-1998_03