A method for preparing 3-(3,5-dichlorophenyl)-2,4-imidazolidinedione
A technology of imidazolidinedione and dichlorophenyl, which is applied in the field of preparation of 3--2,4-imidazolidinedione, can solve the problems of complex process, low yield and high imidazolidinedione yield, and achieves The raw materials are cheap and easy to obtain, the production cost is reduced, and the yield is improved.
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[0017] The invention provides a preparation method of 3-(3,5-dichlorophenyl)-2,4-imidazolidinedione, the 3-(3,5-dichlorophenyl)-2,4-imidazole Alkanediones have a structure shown in formula (I), and the method comprises the following steps:
[0018] (1) Under the condensation reaction conditions, in the presence of a condensation reaction catalyst and an organic solvent, one or more of the compounds represented by the formula (III) is contacted with the compound represented by the formula (II), and the compound containing the formula (IV) mixtures of compounds;
[0019] (2) Under the ring-closing reaction conditions, the mixture containing the compound represented by formula (IV) is directly or separated from the compound represented by formula (IV) and contacted with the ring-closing reaction catalyst;
[0020]
[0021] where, where, R is R 1 , R 1 M 1 or M 2 , R 2 for R 1 or M 2 , where R 1 for C 1 -C 4 The alkyl, preferably methyl, M 1 is hydrochloric acid, su...
preparation example 1
[0056] Add solid phosgene (13.8g, 0.046mol) (purchased from Zhejiang Lishui Youbang Chemical Co., Ltd., purity 99%, the same below) and toluene (60g) into a 250mL reaction bottle, slowly add 3,5-dichloroaniline dropwise (16.2g, 0.1mol) (purchased from Jiangxi Heyi Chemical Co., Ltd., purity 99%, the same below) and triethylamine (1.0g, 0.01mol) (purchased from Beijing Chemical Reagent Company, purity 99%, the same below) Toluene (40.0g) solution, the dropwise addition temperature is controlled at 48±2°C, and the dropwise addition is completed in about 45min. The temperature was raised to 75° C. and kept for 4 hours. Then continue to heat up to 110°C and keep it warm for 3 hours, take samples and monitor until the content of 3,5-dichloroaniline is less than 0.5%, cool down to 60°C, and pass nitrogen gas to remove excess phosgene and hydrochloric acid gas generated by the reaction. That is, toluene solution A1 of 3,5-dichlorophenylisocyanate (114.5 g, w / w=15.7%) was obtained, w...
preparation example 2
[0058]Add solid phosgene (12.0g, 0.04mol) and toluene (100g) into a 250mL reaction flask, slowly add 3,5-dichloroaniline (16.2g, 0.1mol) and triethylamine (1.0g, 0.01mol) dropwise Toluene (40.0g) solution, the dropping temperature is controlled at 48±2°C, and the dropping is completed in about 45 minutes. The temperature was raised to 75° C. and kept for 4 hours. Then continue to heat up to 110°C and keep it warm for 3 hours, take samples and monitor until the content of 3,5-dichloroaniline is less than 0.5%, cool down to 60°C, and pass nitrogen gas to remove excess phosgene and hydrochloric acid gas generated by the reaction. That is, a chlorobenzene solution A2 of 3,5-dichlorophenylisocyanate (156.0 g, w / w=11.5%) was obtained, with a yield of 95.4%.
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