関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Methyl 3,5-Dibromobenzoate | HCID 621923 | — |
| 反応物 | 2-[(1E)-3-methoxyprop-1-en-1-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 16217443 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl 3,5-bis[(1E)-3-methoxyprop-1-en-1-yl]benzoate | HCID 57456870 | — |
反応手順
To a solution of methyl 3,5-dibromobenzoate (1 eq.) from the previous step in DMF (0.2 M) was added 2-[(1E)-3-methoxyprop-1-en-1-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (2.1 eq.), palladium acetate (10 mol %), triphenylphosphine (30 mol %), and 2.0 M aqueous sodium carbonate solution (5 eq.). The reaction was heated to 80° C. and stirred for 3 h. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with water, brine, dried over MgSO4, and concentrated in vacuo. The crude product was purified by flash column chromatography (SiO2, 20% EtOAc in Hex) to afford the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08076359B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
|---|
| ORD ID | ord-d53dca1151d34266a90db378e16b3d56 |
|---|
| 出典メモ | uspto-grants-2011_12 |
|---|
