Preparation method of 3-methyl-4-nitrobenzoic acid

A technology of nitrobenzoic acid and methyl, which is applied in the field of preparation of antihypertensive drug telmisartan intermediates, can solve the problems of low technical selectivity and low conversion rate, and achieve stable reaction, easy control, and conditions mild effect

Inactive Publication Date: 2021-10-08
安徽江泰新材料科技有限公司
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Abstract

The invention relates to a preparation method of 3-methyl-4-nitrobenzoic acid, which comprises the following steps: by taking 2,4-dimethyl nitrobenzene as an initial raw material, carrying out selective oxidation on 4-position methyl to generate 3-methyl-4-nitrobenzoic acid. Compared with the prior art, the method is characterized in that the oxidation comprises the steps of introducing oxygen under stirring and illumination in the presence of an acetonitrile solvent and a catalyst, conducting reacting for 5 hours at the temperature of 30 DEG C, conducting filtering after the reaction is finished, taking filtrate, carrying out rotary evaporation to recover an acetonitrile solvent, adding water, conducting acidifying until the pH is about 3.8, and conducting filtering to obtain 3-methyl-4-nitrobenzoic acid. The conversion rate of 2,4-dimethyl nitrobenzene is greater than or equal to 98%, and the yield of the 3-methyl-4-nitrobenzoic acid is about 65%. The method is mild in condition, stable in reaction, stable in quality, simple in process and convenient to operate.

Application Domain

Organic chemistryOrganic compound preparation

Technology Topic

NitrobenzeneNitrobenzoic acid +6

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  • Preparation method of 3-methyl-4-nitrobenzoic acid

Examples

  • Experimental program(1)

Example Embodiment

[0012] (1) Preparation of 3-methyl-4-nitrobenzoic acid
[0013] 1. Acettonitrile 300ml is added to the photoreceptor (filter tube with filter and except for less than 380 nm), blowing oxygen from below, then adding 2,4-dimethyl nitrobenzene 5g, catalyst hematoporphin 380 mg, NiO 2G The high pressure mercury lamp, 50 ° C reaction for 5 h, filtration, filtration, purifying the solvent acetonitrile, stirred, stirred, acidified to pH = 3.8, filtered to give 3-methyl-4-nitrobenzoic acid 3.95 g, purity 96.7 %.
[0014] 2, the photoreactor (filter tube with filtering with filtering wavelength is less than 380 nm), adding acetonitrile, blowing oxygen from below, then adding 2,4-dimethyl nitrobenzene 5g, catalyst hematoporphyrol monomethyl ether 395 mg NiO 2G, opened high-pressure mercury lamp, 50 ° C reaction for 5 h, filtration, filtration, and evaporation of solvent acetonitrile, residue poured into water, acidified to pH = 3.8, filtered to give 3-methyl-4-nitrobenzoic acid 4.02g , Purity 95.8%.

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