Olivetol CAS 500-66-3

Add 156g benzene, 900mL dichloromethane and 146.5g anhydrous aluminum trichloride into a 2L three-necked flask, cool down to 0-5°C, slowly add 120.5g n-valeryl chloride dropwise, keep the internal temperature 0-10 °C. After the dropwise addition, the temperature was raised to 40 °C, and the reaction was stirred for 2 h.

Under ice bath cooling, 500 mL of 1N hydrochloric acid solution was slowly added dropwise, and the solution was separated after the dropwise addition was completed. The aqueous phase was extracted with an additional 400 mL of DCM. After combining the organic phases, concentrate under reduced pressure and distill to obtain 142 g of valerophenone with a yield of 87%.

In a 1L three-necked flask, 200mL of fuming nitric acid and 200mL of 5% sulfuric acid were mixed within 20°C to form a mixed acid, then cooled to within 10°C, and 129.6g of valerophenone was slowly added dropwise. The dropwise addition process controlled the internal temperature to 0-10°C. After the dropwise addition was completed, the temperature was raised to 50° C. for 2 hours, and the reaction was continued for 5 hours.

After cooling to 20°C, the reaction solution was poured into crushed ice, a solid was precipitated, filtered, the filter cake was dissolved in DCM, and the liquid was separated, and the organic phase was concentrated again to obtain a crude product. The crude product was mixed with PE and EA to dissolve the crystals and dried to obtain 156.5 g of 3,5-dinitrovalerophenone, with a yield of 78% and a purity of 98.3%.