4-Bromo-2-nitroaniline → 4-Bromobenzene-1,2-diamine
반응식
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([N+:9]([O-])=O)[CH:3]=1>[Pt].C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:6])=[CH:7][CH:8]=1참가 물질
4
실험 절차
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).
후처리
- customThe hydrogenation reaction mixture
- filtrationThe reaction mixture was filtered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-ce912197d0244875aab6c2cd6dc5c11e
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07094790B2
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