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With hydrogen bromide; sodium nitrite;copper(I) chloride; In water;
Example 3 [Preparation of 5-bromoisophthalic acid] Into a 1 liter four-necked flask equipped with a thermometer, a stirrer and a dropping funnel, 99.18 g (0.55 moles) of 5-hydroxyisophthalic acid, 165 ml of a 48percent by weight hydrobromic acid and 150 ml of distilled water were placed and the resultant mixture was stirred. The flask was cooled at a temperature of 5OEC or lower. To the cooled mixture, a solution prepared by dissolving 39.4 g (0.57 moles) of sodium nitrite into 525 ml of distilled water was added dropwise over 1 hour and an aqueous solution of a diazonium salt was obtained. Into a 3-liter four-necked flask equipped with a thermometer, a Dimroth condenser, a dropping funnel and a stirrer, 94.25 g (0.66 moles) of cuprous chloride and 45 ml of a 48percent by weight hydrobromic acid were placed and the resultant mixture was stirred. The flask was cooled at a temperature of 0OEC or lower and the aqueous solution of the diazonium salt prepared above was added dropwise over 2 hours. After the addition was completed, the resultant mixture was stirred at the room temperature for 30 minutes and heated for 30 minutes under the refluxing condition. After the reaction mixture was cooled by being left standing, the formed precipitates were separated by filtration and washed twice with 2 liters of distilled water. The obtained white solid substance was dried under a reduced pressure at 50OEC for 2 days and 117 g of a crude product was obtained. The obtained crude product was used for the next step without purification.
With copper(I) oxide; sodium hydroxide; In water; at 130℃; for 20h;
Arranged with the magnetic to the 250 ml round-bottom flask, add 5 - between bromine benzene phthalic acid (20 g, 80 mmol), water (64 ml) and sodium hydroxide (16 g, 400 mmol). Further to this mixed solution of a catalytic amount of cuprous oxide (0.5 g). Then raising the temperature to 130 °C, reflux about 20 h. TLC tracking reaction, after the reaction is complete. The reaction solution was transferred to a dropping funnel, slowly drop added to the citrate 15percent HCl (82 ml) of 250 ml round bottom flask, adding while stirring, white solid precipitated. Mixed solution to rise to 60 - 70 °C, stirring 1 h. Cooling to room temperature, filtered, the filter cake is water (200 ml) washing 3 times. After drying, to obtain white solid 12.8 g, yield 86percent. The product can be directly used for the next step reaction.
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