関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxide (P4O10) | HCID 14812 | — |
| 反応物 | N-(2-phenylpropyl)-4-(trifluoromethyl)benzamide | HCID 24636638 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Methyl-1-(4-(trifluoromethyl)phenyl)-3,4-dihydroisoquinoline | HCID 59536412 | — |
反応手順
A 250-mL round-bottomed flask was charged with N-(2-phenylpropyl)-4-(trifluoromethyl)benzamide (5.19 g, 16.9 mmol), phosphorous pentoxide (4.8 g, 33.8 mmol) and toluene (75 mL). The reaction mixture was heated at 110° C. overnight and allowed to cool down to RT. Then it was poured over ice-water and neutralized with NaOH (10%). The organic phase was separated and the aqueous phase was extracted several times with EtOAc. The combined organics were washed with satd. NaHCO3, water, brine and dried over Na2SO4. The solvent was removed under vacuum and the product used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476297B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-8718eb3ae0a34fa1baec7f00e89daf85 |
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| 出典メモ | uspto-grants-2013_07 |
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