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Methylhydrazine → 2,4,5,6-Tetrahydro-2-methyl-6-(4-nitrobenzoyl)-pyrazolo[4,3-d][1]benzazepin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylhydrazine | HCID 6061 | — |
| 反応物 | 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one | HCID 53653564 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,4,5,6-Tetrahydro-2-methyl-6-(4-nitrobenzoyl)-pyrazolo[4,3-d][1]benzazepin | HCID 57113393 | — |
反応手順
A solution of 0.150 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one and 44 μl of methylhydrazine in 5 ml of methyl alcohol is heated at reflux for 18 hours. A precipitate forms on standing. The volatiles are evaporated to a residue which is purified by column chromatography on silica gel by elution with 5% ethyl acetate-methylene chloride. The product fractions are combined and the volatiles evaporated to a residue which is dissolved in chloroform-methanol, filtered through glass wool and the filtrate evaporated in vacuo to give 0.110 g of the desired product as pale yellow crystals.
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-f2441699a4154e82a18ddbb00b69d577 |
| 出典メモ | uspto-grants-1998_11 |