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6,11Dihydro-5-(4-nitrobenzoyl)-5H-dibenz[b,e]azepine → 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 6,11Dihydro-5-(4-nitrobenzoyl)-5H-dibenz[b,e]azepine | HCID 54499077 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine | HCID 15410467 | 97.4% |
反応手順
To a solution of 4.5 g of 6,11-dihydro-5-(4-nitrobenzoyl)-5H-dibenz[b,e]azepine in 230 ml of glacial acetic acid is added 0.58 g of 10% palladium-on-carbon and the mixture under hydrogen (38 psi) shaken in a Parr hydrogenator for 6.5 hours. The mixture is filtered through diatomaceous earth and the filtrate concentrated to give 4.0 g of solid. The solid is extracted with 100 ml of dichloromethane and the extract washed with water, dried (Na2 SO4). The solvent is removed to give 4.0 g of yellow crystals, m.p. 168°-175° C. A sample chromatographed on a thick layer silica gel plate with hexane-ethyl acetate (8:7) as solvent gives yellow crystals, m.p. 173°-175° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834461 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-bbbbf35c6c3d48d3995babe56996e12d |
| 出典メモ | uspto-grants-1998_11 |