反応 #2329

反応方程式

Bromine

product

methyl 4-(2,2-dimethylacetyl)-phenoxyacetate

→

methyl 4-(2-bromo-2,2-dimethylacetyl)phenoxyacetate

溶媒

carbon tetrachloride

反応条件

後処理

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

実験手順

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).

出典