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Acetamidine monohydrochloride → 6,7-dihydro-2-methyl-7-(4-nitrobenzoyl)-5H-pyrimido[5,4-d][l]benzazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetamidine monohydrochloride | HCID 67170 | — |
| 反応物 | 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one | HCID 53653564 | — |
| 反応物 | HCID 178418582 | HCID 178418582 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6,7-dihydro-2-methyl-7-(4-nitrobenzoyl)-5H-pyrimido[5,4-d][l]benzazepine | HCID 54379793 | 99.7% |
反応手順
To a stirred solution of 0.233 g of acetamidine hydrochloride in 36 ml of methyl alcohol under argon is added 0.133 g of NaOCH3. After 5 minutes, 0.600 g of 4-[(dimethylamino)methylene]-1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one is added and stirring continued for 18 hours. The volatiles are evaporated to a residue which is dissolved in ethyl acetate and passed through a pad of silica gel. The filtrate is evaporated in vacuo to give 590 mg of the desired product as tan crystals, m.p. 211°-212° C. HR FABMS: Exact mass (M+H):361.1295.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05869483 |
| 出典データセット | uspto-grants-1999_02 |
| ORD ID | ord-a0fa1fe4d0924359a6a946b2649fe97b |
| 出典メモ | uspto-grants-1999_02 |