Preparation and application of 2-nitrophloroglucinol_Kain Industrial Additive

Background and overview^[1]

2-Nitrophloroglucinol can be used as a pharmaceutical synthesis intermediate. If 2-nitrophloroglucinol is inhaled, move the patient to fresh air; if the skin comes in contact, take off contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel uncomfortable; if the eyes are clear, In case of contact, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.

Preparation and Application^[1]

2-Nitrophloroglucinol can be used as a pharmaceutical synthesis intermediate. 1,3-phloroglucinol is nitrated using conventional methods to obtain 2-nitrophloroglucinol. In a solution consisting of 33g iodoethane, 29g potassium carbonate and 30ml N,N-dimethylacetamide, 12g of the obtained 2-nitrophloroglucinol was reacted at 80°C for 5 hours. Then, it was poured into 300 ml of water, and the precipitated solid was filtered and washed with water to obtain 13.4 g of 2-nitro-1,3,5-triethoxybenzene. At 90°C, add 12.8g 2-nitro-1,3,5-triethoxybenzene, 28g iron powder and ammonium chloride aqueous solution (2.85g water 8.4ml) into 80ml isopropyl alcohol. The reaction was carried out for 2 hours, extracted with ethyl acetate, the solvent was distilled off, 6 ml of concentrated hydrochloric acid was added, and the mixture was washed with a small amount of acetone to obtain 4.7 g of 2,4,6-triethoxyaniline hydrochloride. This is. Dissolve 2.6 g of 2,4,6-triethoxyaniline hydrochloride in 50 ml of methanol, acidify with 3.5 ml of concentrated hydrochloric acid, and slowly cool the sodium nitrite aqueous solution (1.4 g, 10 ml aqueous solution) with ice to increase the . After 2 hours, add 2.5g sodium methyl sulfate and 2ml concentrated hydrochloric acid. After 1 hour, extract with dichloromethane, wash with water, and evaporate the solvent to obtain 3.0g of light yellow salt.