3,6-dibromo-4,5-difluoro-1,2-phenylenediamine synthesis
- Product Name:3,6-dibromo-4,5-difluoro-1,2-phenylenediamine
- CAS Number:1345627-73-7
- Molecular formula:C6H4Br2F2N2
- Molecular Weight:301.91
1283598-32-2
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1345627-73-7
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Yield:1345627-73-7 89%
Reaction Conditions:
with iron;acetic acid at 45; for 6 h;Inert atmosphere;
Steps:
4 2.2.4 3,6-Dibromo-4,5-difluorobenzene-1,2-diamine (4)
In a 250mL two-neck round-bottom flask, 1,4-dibromo-2,3-difluoro-5,6-dinitrobenzene 3 (3.3g, 9.2mmol), iron powder (7.3g, 130mmol) and acetic acid (130mL) were stirred at 45°C for 6h under argon protection. The solution was cooled down to room temperature and poured into cold 5% NaOH solution (400mL). Then ethyl acetate was added to extract the organic part three times. The ethyl acetate phase was washed with NaHCO3 solution, dried with anhydrous MgSO4, and then the solvent was removed under vacuum to yield 2.5g (89%) of the product as light yellow powder. 1H NMR (300MHz, DMSO) δ (ppm): 5.16 (s, 4H). 13C NMR (75MHz, DMSO) δ (ppm): 141.07, 140.83, 137.97, 130.06, 130.04, 94.65, 94.50, 94.36.
References:
Liu, Xuncheng;Cai, Ping;Chen, Zhenhui;Zhang, Lianjie;Zhang, Xiaofei;Sun, Jiangman;Wang, Haitao;Chen, Junwu;Peng, Junbiao;Chen, Hongzheng;Cao, Yong [Polymer,2014,vol. 55,# 7,p. 1707 - 1715]
1295502-53-2
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$58.00/250mg
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867366-94-7
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$956.12/5g
1345627-73-7
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367-11-3
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$10.00/1g
1345627-73-7
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156682-52-9
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$9.00/1g
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