Preparation method of 3-hydroxyanthranizoic acid hydrochloride_Kain Industrial Additive

Background and overview^[1]

3-Hydroxyanthranilic hydrochloride can be used as a pharmaceutical synthesis intermediate.

Preparation^[1]

The preparation of 3-hydroxyanthranilic acid hydrochloride is as follows: Penicillium is used to catalyze the preparation of 3-hydroxyanthranilic acid, and the reaction formula is as follows:

The substrate 2-aminophenol (1) is reacted catalyzed by Penicillium to obtain the product 3-hydroxyanthranilic acid (2). There are a variety of microorganisms that can catalyze this reaction. After extensive experimental screening, it was finally determined to use Penicillium as the catalyst because it has the best catalytic reaction effect, very few by-products, and a high reaction yield. The specific steps are as follows: 15L fermentation tank, that is, prepare a microbial fermentation liquid fermentation tank. Add the substrate 2-aminophenol to the fermentation liquid to make the concentration 90-95g/L. Add the following ingredients to make the concentration: linear 10-carbon alcohol polyoxyethylene ether is 10-12g/L, xylose 20-24g/L, sucrose 25-28g/L, glutinous rice flour 18-22g/L, autoclave at 121°C for 30 minutes; cool to 33-35 ℃, stir and emulsify, and perform biocatalytic reaction. The reaction time is 49-54 hours; when the reaction starts, immediately add a 5% NaHCO3 aqueous solution, and at the same time, add a 1% hydrochloric acid aqueous solution to adjust the NaHCO3 and hydrochloric acid aqueous solutions. The flow acceleration rate is maintained at pH 6.4-6.6, and the added materials have been sterilized; the ventilation ratio is 0.6-0.7V/V, that is, the ventilation volume per minute is 0.6-0.7 times the volume of the reaction solution. After the reaction is completed, Demulsify, extract the reaction solution three times with 0.2 times the volume of the reaction solution with ethyl acetate, combine the organic phases, and evaporate the ethyl acetate from the organic phase to obtain the product 3-hydroxyanthranilic acid. The reaction conversion rate is 98.1-99.6%. The product The yield is 95.9-97.1%. 3-hydroxyanthranilic acid is further reacted with hydrochloric acid to produce 3-hydroxyanthranilic acid hydrochloride.