関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Cyclopentanepropanol | HCID 69842 | — |
| 反応物 | 4-Hydroxy-3-methoxyphenylacetonitrile | HCID 78220 | — |
| 反応物 | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(4-(3-Cyclopentylpropoxy)-3-methoxyphenyl)acetonitrile | HCID 118389365 | 96.3% |
反応手順
2-(4-Hydroxy-3-methoxyphenyl)acetonitrile (0.54 g, 3.31 mmol) in THF (10 mL) was treated with 3-cyclopentylpropan-1-ol (0.424 g, 3.31 mmol), triphenylphosphine (1.128 g, 4.3 mmol) and cooled in an ice bath to 0° C. DIAD (0.785 ml, 4 mmol) was added to the reaction mixture dropwise over the period of 5 min, and the reaction was left stirring slowly warming to room temperature over 18 hours. The reaction mixture was concentrated. Purification by flash chromatography (silica gel, 0-40% EtOAc/hexanes) afforded 0.871 g (96%) of 2-(4-(3-cyclopentylpropoxy)-3-methoxyphenyl)acetonitrile. MS (ESI) m/z 274 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09284272B2 |
|---|
| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-f40af98d19064883b29c457bc30d1125 |
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| 出典メモ | uspto-grants-2016_03 |
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