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Methanesulfonic Acid → 4-[2-(1-Methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Alpha-Methylstyrene | HCID 7407 | — |
| 反応物 | 4-(1H-1,2,3,4-tetrazol-5-yl)benzaldehyde | HCID 2760606 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-[2-(1-Methyl-1-phenyl-ethyl)-2H-tetrazol-5-yl]-benzaldehyde | HCID 18369100 | — |
反応手順
Under a nitrogen atmosphere, a solution of 6.9 g (58 mmol) of 2-phenyl-propene (Fluka, Buchs, Switzerland) and 22 ml of toluene is added dropwise to 10 g (57 mmol) of 4-(tetra-zol-5-yl)-benzaldehyde and 1 g (5.7 mmol) of methanesulfonic acid in 44 ml of boiling toluene and the mixture is then stirred under reflux conditions for 1 hour. The cooled reaction mixture is washed 2× with sat. NaHCO3 solution, water and brine, dried (Na2SO4) and concentrated by evaporation to form the title compound: 1H-NMR (DMSO-d6) δ 10.09 (s, HCO), 8.29 and 8.08 (2d, J=8, each 2H), 7.33 and 7.17 (2m, 5H), 2.17(S, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06166004 |
| 出典データセット | uspto-grants-2000_12 |
| ORD ID | ord-68e47353f4d4441fb7dc8ed4fed5dfa8 |
| 出典メモ | uspto-grants-2000_12 |