化工社化工社 化学情報印刷レポート · 研究参考用
Azobisisobutyronitrile → Methyl 2-(2-chloro-4-bromomethylphenoxy)-2-phenylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | Methyl 2-(2-chloro-4-methylphenoxy)-2-phenylacetate | HCID 19385673 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | Methyl 2-(2-chloro-4-bromomethylphenoxy)-2-phenylacetate | HCID 19385604 | 34% |
反応手順
To a solution of 1.70 g (5.86 mmol) of the product from Step A dissolved in 20 mL of CCl4 was added 1.04 g (5.86 mmol) of N-bromosuccinimide and 50 mg (catalytic amount) of AIBN. The reaction mixture was stirred and heated at reflux for 7 hours, then an additional 0.20 g of NBS was added. The reaction was refluxed for 48 hours, then cooled and concentrated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 10% ethyl acetate/hexane to afford 0.730 g (34%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05264439 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-0ce25468c7a74d1085cd505e33e7bf69 |
| 出典メモ | uspto-grants-1993_11 |