2,4-DIFLUORO-5-NITROBENZOIC ACID synthesis
- Product Name:2,4-DIFLUORO-5-NITROBENZOIC ACID
- CAS Number:153775-33-8
- Molecular formula:C7H3F2NO4
- Molecular Weight:203.1
1583-58-0
153775-33-8
Step A: 2,4-difluorobenzoic acid (9.985 g, 63.2 mmol) was suspended in concentrated sulfuric acid (30 mL) at 0 °C and fuming nitric acid (30 mL) was slowly added dropwise for 30 minutes. The reaction mixture was then warmed to room temperature and stirring was continued for 16 hours. Upon completion of the reaction, the homogeneous reaction mixture was carefully poured into ice water and extracted with ethyl acetate. The organic phases were combined, washed sequentially with water, dried and finally concentrated under reduced pressure to afford 2,4-difluoro-5-nitrobenzoic acid (12.56 g, 98% yield) as a light yellow solid.
1583-58-0
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153775-33-8
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Yield: 98%
Reaction Conditions:
with sulfuric acid;nitric acid at 0 - 20; for 16.5 h;
Steps:
A
Step A To a suspension of 2,4-difluorobenzoic acid (9.985 g, 63.2 mmol) in concentrated sulfuric acid (30 mL) at 0° C. was added fuming nitric acid (30 mL) over 30 min. The mixture was allowed to warm to RT and stirred for an additional 16 h. The homogeneous mixture was poured onto ice and extracted with ethyl acetate. The organic extract was washed with water, dried and concentrated in vacuo to afford 2,4-difluoro-5-nitrobenzoic acid (12.56 gm, 98%) as pale yellow solid.
References:
Borzilleri, Robert M.;Bhide, Rajeev S.;Tokarski, John S.;Zheng, Peter;Qian, Ligang;Cai, Zhen-Wei US2004/77696, 2004, A1 Location in patent:Page/Page column 9