Preparation of 5-fluoro-2-methylbenzene phenyl-sulfhydrate
A technology of methyl thiophenol and process method, which is applied in the field of preparation of 5-fluoro-2-methyl thiophenol, can solve the problems of limited application, low final yield, high cost of raw materials, etc., and achieves simple conditions , low price, mild reaction effect
Active Publication Date: 2011-09-21
江西豫章药业有限公司 +1
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Problems solved by technology
At present, there is no perfect and mature preparation process for this compound in China. Due to the high cost of raw materials used in the substitution reaction, and the final yield is not very high, the application is limited to a certain extent.
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Embodiment 1
[0012] 1. Preparation of Diazonium Salt
[0013] First, 250 ml of water was added to a 1000 ml three-neck flask, slowly poured into 130 ml (30%) hydrochloric acid, and then slowly added dropwise 62.5 g of 5-fluoro-2-methylaniline. After stirring for 0.5 hours, it was cooled to below -5°C. NaNO was added dropwise to the above solution 2 solution (from 40 g NaNO 2 and 90ml of water). The temperature was controlled between -10 and -5°C, and the dropwise addition was completed in about 1 hour.
[0014] 2. Preparation of intermediate product 5-fluoro-2-methylthiophenate sodium
[0015] Add 108 grams of xanthate and 150 milliliters of water into a 1000 ml three-neck flask, heat it to about 40°C, and then add dropwise the diazonium solution prepared in step 1 into the xanthate solution. Control the temperature between 40-45°C, complete the dropwise addition in about 40 minutes, and control the temperature at about 45°C for 3 hours. After the reaction was completed, the liquid w...
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Abstract
The present invention relates to a method for preparing 5-fluorin-2-methyl benzol thiophenol, characterized in that diazo-reaction is firstly carried out: 250ml of water is added into a three-neck flask with the volume of 1000ml, 130ml of hydrochloric acid is slowly poured into the water and is slowly dripped with 62.5g of 5-fluorin-2-methylaniline, and the mixture is stirred for 0.5 hour to be cooled to the temperature of below -5 DEG C; then NaNO2 solution (which is prepared by 40g of NaNO2 and 90ml of water) is dripped into the obtained solution, and the temperature is controlled within the range of -10 DEG C to -5 DEG C; after that displacement reaction is carried out by airpotato yam which is strong nucleophile, and the product is hydrolyzed to generate 5-fluorin-2-methyl benzol thiophenol sodium in the alkalescent environment; finally, the target product 5-fluorin-2-methyl benzol thiophenol is obtained by acid regurgitation. The method has the advantages that the reaction materials have lower price and are more easily obtained; and the reaction is mild; the reaction condition is simple and stable, thus facilitating large scale production.
Description
technical field [0001] The invention relates to a preparation method of thiophenol, in particular to a preparation method of 5-fluoro-2-methylthiophenol. Background technique [0002] 5-Fluoro-2-methylthiophenol is a colorless or light yellow liquid with a boiling point of 62°C at 55 mmHg. It is the basic raw material for the synthesis of organic compounds such as thiochromanone derivatives. It is expected to become a new high-efficiency, low-efficiency Raw materials and intermediates of toxic and cheap antifungal drugs. There are not many studies on this compound at home and abroad, and it is generally synthesized by diazotization reaction and potassium ethyl xanthate substitution reaction. At present, there is no perfect and mature preparation process for this compound in China. Due to the high cost of raw materials used in the substitution reaction, and the final yield is not very high, the application is limited to a certain extent. In view of this fact, the present in...
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IPC IPC(8): C07C323/09C07C319/02
Inventor 谢宇胡金刚
Owner 江西豫章药业有限公司