Synthesis of 1,3-terahydro thiazolone compound
A technology of tetrahydrothiazolone and tetrahydrothiazolethione, applied in 1, can solve the problems of high price and difficult application of dioxane, and achieve the effect of large commercial application value, improvement of purity and quality, reduction of requirements and costs
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example 1
[0015] Toluene was used as the reaction solvent. 119 g of 1,3-tetrahydrothiazolthione-2 (II, R=H), 48 g of ethylene oxide and 500 ml of toluene were placed in a closed reactor and reacted at ~80°C for 6 hours. After the reaction was completed, the low boiling point was distilled off, filtered, and then the toluene was distilled off, and the residue was recrystallized with toluene to obtain 61 grams of a white crystal product, with a melting point of 52.5-54° C. and a compound (I) content (GC method) of 99.1% in the product .
example 2-5
[0017] Operation method is the same as example 1, and the reaction solvent adopts benzene, acetonitrile, dimethyl sulfoxide and butanone respectively, and the results are basically the same.
example 6
[0019] Ethanol was used as the reaction solvent. Add 119 g of 1,3-tetrahydrothiazolthione-2 (II, R=H) into 500 ml of ethanol, heat to 50°C to dissolve, and pass ethylene oxide gas at this temperature under stirring for about 2 hours. Add 48 grams of ethylene oxide. After the addition of ethylene oxide was complete, the reaction was heated to reflux under ethanol for 6 hours. After the reaction was completed, the solid was filtered off, the ethanol residue was removed under reduced pressure, and recrystallized with ethanol to obtain 67 grams of a white crystalline product with a melting point of 53-54° C. and a compound (I) content (GC method) of 99.5% in the product.
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