Process for production of iodine compounds and process for production of high-purity 5-iodo-2-methylbenzoic acid
A technology of methylbenzoic acid and compounds, applied in the field of preparation technology of high-purity 5-iodo-2-methylbenzoic acid, can solve the problem of product purity and separation yield damage, which has never been known and has not been shown to reduce regioisometry Questions about the amount of by-products of the conformation
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Embodiment 1
[0074] Example 1: 2-methylbenzoic acid
[0075] Add acetic acid (100 grams), H-beta zeolite (4.6 grams), iodine (20.2 grams, 0.16 moles), 2-methylbenzoic acid (20 grams , 0.15 mol), periodate dihydrate (7.3 g, 0.03 mol) and sulfuric acid (0.24 g), which were mixed well and stirred at room temperature. The temperature of the mixture was raised to 110°C in a heating mantle, after which the reaction was carried out for 1 hour. Then, the reaction was carried out at the reflux temperature of acetic acid (about 118° C.) for 5 hours.
[0076] After the reaction, the reaction mixture was filtered to recover the H-beta zeolite, and 10% by weight aqueous sodium sulfite (100 ml) was added to the filtrate to treat the remaining iodine. Next, water (800 g) was added thereto to precipitate crystals, which were then filtered and recovered.
[0077] The crystals and filtrate thus obtained were analyzed by HPLC (High Pressure Liquid Chromatography) to study the improvement of properties, an...
Embodiment 2
[0080] Example 2: 3-methylbenzoic acid
[0081] The same method as in Example 1 was carried out except that 3-methylbenzoic acid (20 g, 0.15 mol) was used as a reactant. 50% conversion of 3-methylbenzoic acid, 40% yield for 6-iodo-3-methylbenzoic acid 1) and 8% yield for other iodide regioisomers 2); The ratio of 1) / 2) is 5.
Embodiment 3
[0084] Example 3: 2,4-dimethylbenzoic acid
[0085] The same method as in Example 1 was carried out except that 2,4-dimethylbenzoic acid (22.5 g, 0.15 mol) was used as a reactant. 98% conversion of 2,4-dimethylbenzoic acid, 88% yield for 5-iodo-2,4-dimethylbenzoic acid 1) and 2) for other iodide regioisomers The yield was 7%. The ratio of 1) / 2) is 12.6.
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