関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Calcium Chloride | HCID 5284359 | — |
| 反応物 | (4-Methoxy-3-nitro-phenyl)-bis-(4-methyl-benzyl)-amine | HCID 22736971 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-methoxy-N1,N1-bis-(4-methyl-benzyl)-benzene-1,3-diamine | HCID 22736966 | 91.1% |
反応手順
To a stirred solution of 500 mg (1.33 mmol) (4-methoxy-3-nitro-phenyl)-bis-(4-methyl-benzyl)-amine in 20 ml ethanol at room temperature were added 1.91 g (29.2 mmol) zinc powder and 147 mg (1.33 mmol) calcium chloride and the mixture was then heated at 90° C. for 16 hours. The mixture was then filtered and the filtrate diluted with ethyl acetate and washed with 0.5 N sodium hydroxide solution and then with brine. The organic phase was dried over sodium sulfate and concentrated in vacuo to afford 420 mg (91%) 4-methoxy-N1,N1-bis-(4-methyl-benzyl)-benzene-1,3-diamine as a dark brown oil. ES-MS m/e (%): 347 (M+H+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713499B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-bb3f0eeaebb04945a0a5661a68669b85 |
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| 出典メモ | uspto-grants-2004_03 |
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