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Hydrochloric Acid → 3-Methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 4-Methyl-2-(2-nitro-phenylamino)-benzonitrile | HCID 21093529 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-Methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride | HCID 21093523 | 49.2% |
反応手順
Combine 4-methyl-2-(2-nitro-phenylamino)-benzonitrile (2.46 g, 9.71 mmol), tin(II) chloride dihydrate (6.57 g, 29.71 mmol), 5N. HCl (40 ml), and ethanol (40.0 ml). Stir the mixture at reflux for 8 hours then cool it to ambient temperature. Allow the mixture to stand at ambient temperature overnight then chill it for 3 hours in the refrigerator. Remove the resulting precipitate by vacuum filtration and dry it under vacuum to give 1.24 g (49%) of the desired compound as a yellow solid: mass spectrum (ion spray): m/z=224.0 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07214673B2 |
| 出典データセット | uspto-grants-2007_05 |
| ORD ID | ord-cda4d3c906a441dca6161ac9d71f3f22 |
| 出典メモ | uspto-grants-2007_05 |