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Toluene → Methyl 3,5-bis(3-methoxypropyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Benzenesulfonyl hydrazide | HCID 65723 | — |
| 反応物 | Methyl 3,5-bis[(1E)-3-methoxyprop-1-en-1-yl]benzoate | HCID 57456870 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Methyl 3,5-bis(3-methoxypropyl)benzoate | HCID 57456871 | — |
反応手順
To a solution of methyl 3,5-bis[(1E)-3-methoxyprop-1-en-1-yl]benzoate (1 eq.) from the previous step in refluxing toluene was added benzenesulfonohydrazide (5 eq) in five portions over 2 h. The reaction was stirring as reflux for 18 h. After cooling to rt, the reaction was diluted with ether. The organic extract was washed with 1 N aqueous HCl, 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-b1bcb487c77a41f4a782d110b154de33 |
| 出典メモ | uspto-grants-2011_12 |