関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylarsine | HCID 11773 | — |
| 反応物 | Tributylphenyltin | HCID 607632 | — |
| 反応物 | Methyl 2-iodo-5-(methylsulfonyl)benzoate | HCID 59853752 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Methanesulfonyl-biphenyl-2-carboxylic acid methyl ester | HCID 57753217 | 99% |
反応手順
A mixture of 3.53 mmol 2-Iodo-5-methanesulfonyl-benzoic acid methyl ester, 3.88 mmol Phenyltri-n-butyltin, 0.25 mmol Tris(dibenzylideneacetone)dipalladium(0), 0.35 mmol Triphenylarsine and 1.62 mmol Copper iodide in N,N-Dimethylformamide (30 ml) was heated at 90° C. for 16 hours. The mixture was cooled to room temperature and concentrated in vacuo. The residue was chromatographed over SiO2 (ethyl acetate/heptane gradient) to provide the title compound (99%) as an off-white crystalline solid. MS (m/e): 291.0 (MH+, 100%)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07557114B2 |
|---|
| 出典データセット | uspto-grants-2009_07 |
|---|
| ORD ID | ord-080b43447f2e4e1ea5a6295673c01f4d |
|---|
| 出典メモ | uspto-grants-2009_07 |
|---|
