N,2-diMethyl-5-nitroaniline synthesis
- Product Name:N,2-diMethyl-5-nitroaniline
- CAS Number:10224-71-2
- Molecular formula:C8H10N2O2
- Molecular Weight:166.18
Yield:10224-71-2 60%
Reaction Conditions:
Stage #1: formaldehyd;2-methyl-5-nitroanilinewith sodium methylate in methanol at 20; for 12 h;Inert atmosphere;
Stage #2: with sodium tetrahydroborate in methanol at 20; for 12 h;Inert atmosphere;
Steps:
22.1
Dissolve 22a (3.04g, 20.00mmol), paraformaldehyde (2.40g, 80.00mmol), sodium methoxide (540mg, 10.00mmol) in methanol (100mL), replace with nitrogen three times, stir at room temperature for 12 hours, and then add Sodium borohydride (1.52g, 40.00mmol), replaced with nitrogen three times, stirred at room temperature for 12 hours, directly concentrated under reduced pressure to obtain a residue, and the residue was purified by column chromatography (ethyl acetate: petroleum ether=0-100%) 22b (2.00g), yield: 60%.
References:
CN112300069,2021,A Location in patent:Paragraph 0401-0405
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