5-methyl-3-nitrobenzene-1,2-diol synthesis
- Product Name:5-methyl-3-nitrobenzene-1,2-diol
- CAS Number:89791-96-8
- Molecular formula:C7H7NO4
- Molecular Weight:169.13
53411-80-6
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89791-96-8
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Yield:89791-96-8 81%
Reaction Conditions:
with tetrabutyl ammonium fluoride;hydrogen bromide in water at 110; for 18 h;Concentration;
Steps:
6.4 (2) Preparation of 5-methyl-3-nitrobenzene-1,2-diol
2-Methoxy-4-methyl-6-nitrophenol (20.0 g, 0.109 mol) was added to 150mL hydrobromic acid (80%), and 15g tetrabutylammonium fluoride was added. The resultant mixture was heated to 110°C and reacted for 18 h. After thereaction, 800mL water was added. After extraction with ethyl acetate (53400mL), the organic phases were combined,washed with saturated NaCl aqueous solution (250mL), dried with anhydrous sodium sulphate, and filtrated. The solventwas removed by rotary evaporation, and the residue was subjected to silica gel column chromatography (petroleumether: ethyl acetate= 5:1) to obtain the product (15 g, yield: 81%).
References:
EP3202765,2017,A1 Location in patent:Paragraph 0168; 0169; 0191; 0192; 0222; 0223
452-86-8
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93-51-6
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$15.00/5g
89791-96-8
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1688-19-3
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