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p-Xylyl bromide → (4-Methoxy-3-nitro-phenyl)-bis-(4-methyl-benzyl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Xylyl bromide | HCID 7721 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Benzenamine, 4-methoxy-3-nitro- | HCID 123071 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (4-Methoxy-3-nitro-phenyl)-bis-(4-methyl-benzyl)-amine | HCID 22736971 | 93% |
反応手順
To a stirred solution of 5.00 g (29.7 mmol) 4-methoxy-3-nitro-phenylamine in 60 ml acetonitrile at 0° C. were added 10.2 ml (59.5 mmol) N-ethyldiisopropylamine and 11.6 g (62.4 mmol) 4-methylbenzyl bromide. Stirring was continued at room temperature for 16 h and then the mixture was diluted with ethyl acetate and washed with 0.5 N hydrochloric acid and then with brine. The organic phase was dried over sodium sulfate and concentrated in vacuo to afford 10.4 g (93%) (4-methoxy-3-nitro-phenyl)-bis-(4-methyl-benzyl)-amine as an orange oil. ES-MS m/e (%): 399 (M+Na+, 18), 377 (M+H+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713499B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-ff2ffa8c03f24d1283bb8fd94dc8bf7e |
| 出典メモ | uspto-grants-2004_03 |