Preparation method of dichloropyrimidine
A technology of dichloropyrimidine and dihydroxypyrimidine, which is applied in the field of pesticides, can solve the problems of large amount of catalyst, troublesome wastewater treatment, difficult recycling, etc., and achieve the effects of avoiding recycling and reuse, good yield and environmental friendliness
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[0026] The present invention provides a method for preparing dichloropyrimidine, which comprises the following steps:
[0027] 1) in the presence of a catalyst, dihydroxypyrimidine and a chlorinating reagent are made to carry out a chlorination reaction in a solvent;
[0028] 2) separating and obtaining dichloropyrimidine from the reaction product obtained in step 1),
[0029] Wherein, the catalyst is a combination of organic phosphorus and thionyl chloride or an organic base, and the organic phosphine is selected from one of the compound represented by the following formula (1) and the compound represented by the formula (2) or variety,
[0030]
[0031] In formula (1) and formula (2), R 1 , R 2 and R 3 One of each independently selected from the group consisting of an alkyl group having 1-4 carbon atoms, an aryl group having 6-10 carbon atoms, an alkoxy group having 1-4 carbon atoms and an aryloxy group having 6-10 carbon atoms or more;
[0032] The chlorinating rea...
Embodiment 1
[0048] In a device equipped with a reflux condenser, a thermometer and a stirrer, 4,6-dihydroxypyrimidine (114.3 g, 98% by weight, 1 mol), triphenylphosphine (14.1 g, 99% by weight, 0.05 g) were added. mol), thionyl chloride (12.0g, content 99% by weight, 0.1mol) and 1,2-dichloroethane 1000mL, after stirring evenly, the temperature was raised to 75-80°C, and phosgene was slowly introduced into the reaction for 10h After sampling, HPLC analysis of 4,6-dihydroxypyrimidine was 0.4%, and the content of 4,6-dichloropyrimidine was 98.2%, and the reaction was completed. The obtained reaction solution was rectified under vacuum (temperature of 95-130°C, pressure of -0.09-0.095MPa) to obtain 4,6-dichloropyrimidine with a content of 98.1% by weight and a yield of 93.9%.
Embodiment 2
[0050] In a device equipped with a reflux condenser, a thermometer and a stirrer, 4,6-dihydroxypyrimidine (114.3 g, 98% by weight, 1 mol), triphenylphosphine (14.1 g, 99% by weight, 0.05 g) were added. mol), triethylamine (10.2g, content of 99% by weight, 0.1mol) and 1,2-dichloroethane 1000mL, after stirring evenly, the temperature was raised to 75-80°C, and phosgene was slowly introduced to react, after 10h Sampling, HPLC analysis showed that the content of 4,6-dihydroxypyrimidine was 0.1%, and the content of 4,6-dichloropyrimidine was 98.8%, and the reaction was completed. The obtained reaction solution was rectified under reduced pressure to obtain 4,6-dichloropyrimidine with a content of 98.1% by weight and a yield of 94.3%.
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