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Lawesson's reagent → 6,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lawesson's reagent | HCID 87949 | — |
| 反応物 | Dibenz(b,e)oxepin-11-carboxamide, 6,11-dihydro-N-(2,6-bis(1-methylethyl)phenyl)-2-methyl- | HCID 3072807 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6,11-Dihydro-N-(2,6-diisopropylphenyl)-2-methyldibenz[b,e]oxepin-11-carbothioamide | HCID 10455333 | 96.3% |
反応手順
After 1.09 g of Compound 4 obtained in Example 4 was dissolved in 10 ml of toluene, 1.07 g of Lawesson's reagent was added to the solution. The mixture was heated under reflux for an hour. The reaction mixture was allowed to stand at room temperature, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography [eluent: hexane-ethyl acetate (2:1 )]to obtain 1.46 g of a crude product. The crude product was recrystallized from ethyl acetate-hexane to obtain 1.09 g of Compound 36.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05340807 |
| 出典データセット | uspto-grants-1994_08 |
| ORD ID | ord-d8e661bcd65c49a49de6dd8233e94387 |
| 出典メモ | uspto-grants-1994_08 |