Preparation method of symmetric aromatic anhydride compound
A technology for aromatic acid anhydrides and compounds, which is applied in the field of preparation of symmetrical aromatic acid anhydride compounds, can solve the problems of difficult preparation of raw materials, high reaction temperature, and high yield, and achieve good industrial application prospects, mild reaction conditions, and high yield. Effect
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Embodiment 1
[0042] Add 3.3ml (20mmol) α-terpineol, 2.4ml pyridine, 35ml methylene dichloride in the 150ml three-necked flask that condenser tube, thermometer are housed, and the three-necked flask is placed in constant temperature heating magnetic stirrer, open condensed water, Turn on magnetic stirring and heat. When the temperature of the solution rose to 30°C, a solution composed of 3.1 mL (24 mmol) p-chlorobenzoyl chloride and 15 mL of dry dichloromethane was added dropwise through a constant pressure funnel. After the dropwise addition was completed, the reaction was heated to reflux for 16h. After the reaction was over, a large amount of white solids were precipitated in the three-necked flask, and 30 mL of hydrochloric acid (1mol / L) was added to the reaction solution, shaken up and allowed to stand for 1 hour, then suction filtered, and successively with 30 mL of 1.5 mol / L NaOH aqueous solution and 30 mL of distilled water After washing once, and vacuum drying at 75°C, 3.06 g of p...
Embodiment 2
[0046] Add 3.3ml (20mmol) α-terpineol, 2.4ml pyridine, 35ml methylene dichloride in the 150ml three-necked flask that condenser tube, thermometer are housed, and the three-necked flask is placed in constant temperature heating magnetic stirrer, open condensed water, Turn on magnetic stirring and heat. When the temperature of the solution rose to 30°C, a solution composed of 3.2 mL (24 mmol) p-toluoyl chloride and 15 mL of dry dichloromethane was added dropwise through a constant pressure funnel. After the dropwise addition was completed, the reaction was heated to reflux for 16h. After the reaction was over, the reaction solution was extracted once with 30mL hydrochloric acid (1mol / L), 30mL concentration of 1.5mol / L NaOH aqueous solution, and 30mL distilled water, and the organic phase was evaporated in vacuo to obtain 6.15g yellow oil concentrate. Silica gel column chromatography (eluent: 5% ethyl acetate petroleum ether solution) and vacuum drying at 75°C gave 2.82g of p-to...
Embodiment 3
[0050] Add 3.3ml (20mmol) α-terpineol, 2.4ml pyridine, 35ml methylene dichloride in the 150ml three-necked flask that condenser tube, thermometer are housed, and the three-necked flask is placed in constant temperature heating magnetic stirrer, open condensed water, Turn on magnetic stirring and heat. When the temperature of the solution rose to 30°C, a solution consisting of 2.84 mL (24 mmol) of p-fluorobenzoyl chloride and 15 mL of dry dichloromethane was added dropwise through a constant pressure funnel. After the addition is complete, the reaction will be heated to reflux for 8h. After the reaction was finished, the reaction solution was extracted once with 30mL hydrochloric acid (1mol / L), 30mL concentration of 1.5mol / L NaOH aqueous solution, and 30mL distilled water, and the organic phase was rotary evaporated in vacuo to obtain 5.35g yellow oil concentrate, and the yellow oil concentrate was subjected to Silica gel column chromatography (eluent: 5% ethyl acetate petrole...
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