1-bromo-4,5-dimethyl-2-nitrobenzene synthesis
- Product Name:1-bromo-4,5-dimethyl-2-nitrobenzene
- CAS Number:53938-24-2
- Molecular formula:C8H8BrNO2
- Molecular Weight:230.06
99-51-4
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Yield:53938-24-2 89.4%
Reaction Conditions:
with hydrogen bromide;copper(I) bromide;sodium nitrite in water at -5 - 70; for 1 h;
Steps:
1.3 Step 3: 1-Bromo-4,5-dimethyl-2-nitrobenzene
Dissolve 4,5-dimethyl-2-nitroaniline (300.0mg, 1.8mmol) in a mixed solution of distilled water (11.4ml) and HBr solution (48%, 32ml), stir at 70 ° C for 30min, and cool to After -5 ° C, NaNO2 (780.0 mg, 11.3 mmol) was added to an aqueous solution (4 ml). The temperature of the system was kept at -5 ° C for 15 minutes, and a freshly prepared solution of CuBr (3.27 g, 24.3 mmol) in HBr (48%, 6 ml) was added and heated at 70 ° C for 15 minutes. The reaction mixture was extracted three times with dichloromethane (20 ml X 3). The combined organic phases were washed with NaOH (10%, 20 ml), dried over anhydrous NaSO4, filtered, and the solvent was evaporated under reduced pressure. Purification by column chromatography (PE / EA = 9: 1) gave a yellow solid (370.2 mg, 89.4%).
References:
CN110862383,2020,A Location in patent:Paragraph 0054; 0062-0064
6972-71-0
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583-71-1
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$13.43/1gm:
53938-24-2
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