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4-Bromo-2-nitroaniline → 4-Bromobenzene-1,2-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Bromo-2-nitroaniline | HCID 70132 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Bromobenzene-1,2-diamine | HCID 323593 | 103% |
反応手順
4-Bromo-2-nitroaniline (12 g, 55 mmol), 1% Pt/C (1.2 g) and THF (120 mL) were added to a 250 mL bottle. The reaction mixture was hydrogenated at a pressure of approximately 40 psig H2. The hydrogenation reaction mixture was monitored by HPLC until the Area % of 4-bromo-2-nitroaniliine was less than 1%. The reaction mixture was filtered and then concentrated to yield 10.6 g of 4-bromo-benzene-1,2-diamine (as a black oil that solidifies). 4-Bromo-benzene-1,2-diamine was used in the next step without further purification. 1H NMR (400 MHz, CDCl3) δ 3.28 (br, 4H), 6.54 (d, 1H), 6.77–6.81 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094790B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ce912197d0244875aab6c2cd6dc5c11e |
| 出典メモ | uspto-grants-2006_08 |