2-Isobutyl-5-nitrobenzonitrile synthesis
- Product Name:2-Isobutyl-5-nitrobenzonitrile
- CAS Number:288251-96-7
- Molecular formula:C11H12N2O2
- Molecular Weight:204.23
Yield:288251-96-7 56.3%
Reaction Conditions:
with caesium carbonate in water;toluene; for 2 h;Microwave irradiation;Heating;Inert atmosphere;
Steps:
31.1 Step 1:
Synthesis of 2-isobutyl-5-nitrobenzonitrile
To a mixture of 5-amino-2-bromobenzonitrile (1 g, 5.1 mmol), isobutylboronic acid (1.2 g, 11.8 mmol), caesium carbonate (2 g, 6.1 mmol), toluene (10 mL) and water (0.3 mL) in a 20 mL microwave tube was added Pd(dppf)Cl2 (350 mg, 0.48 mmol) under nitrogen atmosphere, and the mixture was heated to react at 120□ under microwave for 2 hours.
After completion of the reaction, solvent was removed in vacuo, then saturated sodium chloride (20 mL) was added.
The mixture was extracted with ethyl acetate (8 mL), dried over anhydrous sodium sulfate.
The organic layers were combined and concentrated in vacuo, and the crude product was separated by a silica gel column (petroleum ether: ethyl acetate = 10:1) to give a product (white solid, 0.5 g), with a yield of 56.3%. MS (ESI) m/z:175.1(M+1).
References:
EP3581561,2019,A1 Location in patent:Paragraph 0179; 0171
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