ChemicalBook CAS DataBase List Methyl 3-methyl-4-nitrobenzoate

Methyl 3-methyl-4-nitrobenzoate synthesis

9synthesis methods

Product Name:Methyl 3-methyl-4-nitrobenzoate
CAS Number:24078-21-5
Molecular formula:C9H9NO4
Molecular Weight:195.17

67-56-1

3113-71-1

24078-21-5

Step 1. Synthesis of methyl 3-methyl-4-nitrobenzoate 3-Methyl-4-nitrobenzoic acid (30 g, 165.61 mmol) was dissolved in methanol (300 mL), stirred at 0°C and thionyl chloride (25 mL) was added slowly and dropwise. The reaction mixture was warmed to 80°C and stirring was continued for 1 hour. Upon completion of the reaction, the mixture was concentrated under reduced pressure to give the crude product. The crude product was dissolved in petroleum ether (100 mL) and filtered to give methyl 3-methyl-4-nitrobenzoate as a white solid (31 g, 96% yield). Product Characterization: LC/MS (ES, m/z): [M + H]+ 196.01 1H-NMR (300MHz, CD3Cl) δ 7.99-8.04 (m, 3H), 3.98 (s, 3H), 2.64 (s, 3H)

67-56-1 Synthesis

67-56-1
782 suppliers
$7.29/5ml-f

3113-71-1 Synthesis

3113-71-1
491 suppliers
$6.00/25g

24078-21-5
249 suppliers
$6.00/5g

Yield:24078-21-5 96%

Reaction Conditions:

with thionyl chloride at 0 - 80; for 1 h;

Steps:

40.1
Step 1. Methyl 3-methyl-4-nitrobenzoate To a solution of 3-methyl-4-nitrobenzoic acid (30 g, 165.61 mmol) in methanol (300 mL), was added thionyl chloride (25 mL) dropwise with stirring at 0° C. After stirring for 1 h at 80° C., the resulting mixture was concentrated under vacuum to give residue, which was dissolved in petroleum ether (100 mL) and filtrated to give methyl 3-methyl-4-nitrobenzoate as a white solid (31 g, 96%). LC/MS (ES, m/z): [M+H]⁺ 196.0 ¹H-NMR (300 MHz, CD₃Cl) δ 7.99-8.04 (m, 3H), 3.98 (s, 3H), 2.64 (s, 3H)

References:

BIOENERGENIX US2012/277224, 2012, A1 Location in patent:Page/Page column 33

FullText