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Sodium hydride → 7-Methyl-2,3-dihydro-1-benzofuran-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Trimethyloxosulphonium chloride | HCID 197819 | — |
| 反応物 | 3-Methylsalicylaldehyde | HCID 522777 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 7-Methyl-2,3-dihydro-1-benzofuran-3-ol | HCID 13013060 | — |
反応手順
Under a nitrogen atmosphere 0.945 g (7.35 mmol) trimethylsulphoxonium chloride were placed in 20 mL THF, and 0.300 g (7.50 mmol) sodium hydride (55%, suspension in mineral oil) were added batchwise. The reaction mixture was refluxed for 2 h. Then 1.00 g (7.35 mmol) 2-hydroxy-3-methylbenzaldehyde in 20 mL THF were added dropwise to the reaction mixture and it was refluxed overnight. Then PE was added and the suspension obtained was filtered. The filtrate was evaporated down i. vac. and purified by flash chromatography. The fractions containing the product were combined and evaporated down.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08629137B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-83e49fa21a4c4926ac8c167607bd148d |
| 出典メモ | uspto-grants-2014_01 |