Process for production of iodine compounds and process for production of high-purity 5-iodo-2-methylbenzoic acid
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A technology of toluic acid and compound, applied in the field of preparation technology of high-purity 5-iodo-2-methylbenzoic acid, can solve the problem of not showing reduction in the amount of by-products of regioisomers, product purity and separation yield Broken, Unknown, etc.
Inactive Publication Date: 2006-03-15
日本精细化工株式会社
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Problems solved by technology
Therefore, the problem involved therein is that product purity and isolation yields are compromised, however, no method to reduce the amount of regioisomer by-products is shown in any of the general methods shown above
A known method for regioselectively separating aromatic compounds is a method of reacting iodine monochloride in the presence of zeolite (Catalysis L
Method used
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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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Abstract
Provided is a production method for an iodine compound in which iodine is reacted with a substrate in the presence of a porous material having a pore diameter of 500 nm or less or in the presence of the above porous material and an oxidizing agent and a production process for high purity 5-iodo-2-methylbenzoic acid comprising an iodination reaction step carried out by the above-mentioned, a crystal precipitation and separation step in which a product is precipitated by adding water or cooling and then separated and a purification step in which crystal separated is recrystallized using an organic solvent. According to the production method for an iodine compound described above, iodine can be introduced into various substrates at a high selectivity. Since expensive metals and specific reagents do not have to be used, it can readily be carried out in an industrially scale, and the product having a high purity can be obtained. Further, the process comprising the iodination reaction, separation and purification steps described above makes it possible to readily obtain at a high yield, 5-iodo-2-methylbenzoic acid having a high purity which is useful in uses for functional chemical products such as medicines. The process of the present invention comprising iodination reaction, separation and purification steps is characterized by that it is simple in terms of a procedure and that the purification load is smaller, and it is very advantageous in industrially carrying out.
Description
Background of the invention [0001] The invention relates to a method for directly and selectively preparing iodine compounds using iodine, and a preparation process for high-purity 5-iodo-2-methylbenzoic acid. Iodine compounds are important compounds that are widely used as medicines such as contrast agents and therapeutic agents for thyroid diseases, hygienic materials for antifungal and antifungal purposes, electronic materials, optical functional materials, etchant, for life Catalysts and materials for chemical reactions in the fields of science, electro-, information-communication, environment and energy. And besides its use as pharmaceuticals and agricultural chemicals, high purity 5-iodo-2-methylbenzoic acid is a useful raw material for various performance chemicals. [0002] related technology [0003] Compounds containing fluorine or iodine atoms have characteristics not observed in other halogen-containing compounds. For example, fluorine atoms are small in size an...
Claims
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