関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 4,5,6,7-Tetrahydro-1-benzofuran-4-one | HCID 2733541 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Decalin | HCID 7044 | — |
| 溶媒 | 1-Dodecene | HCID 8183 | — |
| 生成物 | 4-Benzofuranol | HCID 11607921 | — |
反応手順
3.76 g (27.6 mmol) of 6,7-dihydro-1-benzofuran-4(5H)-one (prepared according to Tetrahedron Lett. 1994, 35, 6231) and 10% of palladium on activated carbon in 34 ml of decalin and 6 ml of dodecene are heated in a metal bath at 200° C. overnight. The mixture is cooled to 80° C., ethanol is added and the mixture is filtered off through CELITE (diatomaceous earth). The CELITE (diatomaceous earth) is washed twice with ethanol and the filtrate is concentrated. The residue, which still contains decalin and dodecene, is mixed with petroleum ether and cooled in an ice bath. An oily precipitate forms. The solvent is decanted off and the oil is purified by preparative HPLC.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07737153B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-e53e6d184e694ac9ab2df5d78b9d045c |
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| 出典メモ | uspto-grants-2010_06 |
|---|
