- Synthesis method of 4,5,6-trichloropyrimidine
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The invention particularly relates to a synthesis method of 4,5,6-trichloropyrimidine. The method comprises the following steps: 1, dissolving diethyl malonate in dichloromethane, adding chlorosuccinimide at room temperature, and reacting to obtain an intermediate diethyl 2-chloromalonate; 2, dissolving sodium methoxide in methanol, cooling to room temperature, adding formamidine hydrochloride, stirring at room temperature after addition, adding the diethyl 2-chloromalonate in a dropwise manner, heating, carrying out a reflux reaction for 2-3 hours after addition, and purifying to obtain an intermediate 5-chloro-4,6-dihydroxypyrimidine; and 3, mixing the intermediate 5-chloro-4,6-dihydroxypyrimidine, phosphorus oxychloride and an organic alkali according to a weight ratio of 1:(5-10):(0.3-2), carrying out a chlorination reaction at 25-100 DEG C for 2-5 hours, cooling the mixture, carrying out reduced pressure concentration to remove redundant phosphorus oxychloride, adding water, quenching, extracting with an organic solvent, drying, and concentrating to obtain the product 4,5,6-trichloropyrimidine.
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Paragraph 0030
(2020/08/02)
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- Method for synthesizing adenine and derivatives thereof
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The invention discloses a method for synthesizing adenine and derivatives thereof. The method comprises the steps: firstly, subjecting diethyl malonate and dimethyl dioxirane to an oxidation reaction, so as to obtain 2-hydroxyldiethyl malonate; then, carrying out an ammonolysis reaction with ammonia water, so as to obtain 2-hydroxyl malonamide; then, carrying out a cyclization reaction with trimethyl orthoformate, so as to obtain 5-hydroxyl pyrimid-4,6-(1H,5H)-dione; then, carrying out a chlorination reaction with phosgene, so as to obtain 4,5,6-trichloropyrimidine; then, carrying out a cyclization reaction with formamidine hydrochloride, so as to obtain 4-chloro-1H-pyrazol[3, 4-d]pyrimidine; finally, carrying out an ammoniation reaction with ammonia water or an amine compound in the presence of triethylamine, thereby obtaining the adenine and derivatives thereof. According to the method, the raw materials are moderately-priced and readily available, the reaction conditions are mild, the reaction process is safe, the requirements on production equipment are low, particularly, the environmental pollution is light, and the yield is relatively high, so that the method is applicable to industrial large-scale production.
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Paragraph 0032; 0039; 0040
(2017/07/19)
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- PROCESS FOR PRODUCING TRICHLOROPYRIMIDINE COMPOUND
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A process for producing a trichloropyrimidine compound represented by the formula (2): wherein R represents a hydrogen atom etc., comprising reacting a dihydroxypyrimidine compound represented by the formula (1): wherein R represents the same meaning as above, with sulfuryl chloride and at least one chlorinating agent selected from the group consisting of hydrogen chloride, thionyl chloride, phosgene, phosphorus oxychloride, phosphorus pentachloride and phosphorus trichloride in the presence of an organic base.
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Page/Page column 7
(2009/12/23)
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- PYRIMIDINE DERIVATIVES AND HERBICIDES CONTAINING THE SAME
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The present invention provides a pyrimidine derivative represented by the formula: wherein R1p and R1q are the same or different, and each represents (1)hydrogen, (2)halogen, (3) a C1-6alkyl group which may be substituted or (4) a C1-6alkoxy group, and so on, R2 is halogen, a C1-6alkyl group, cyano group, and so on, Ar is a phenyl group which may be substituted or is a condensed hetero ring which may be substituted, which has excellent selective herbicidal activity, and a herbicide containing the derivative.
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- Method of preparing 4,5,6-trichloro-and 2,4,5,6-tetrachloropyrimidine
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Crystals with an average crystal size of ≦10 μm comprising compounds of the formula Ia and/or IIa A process for making said crystals.
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- Method of preparing 4,5,6-trichloro- and 2,4,5,6-tetrachloropyrimidine
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PCT No. PCT/EP97/02933 Sec. 371 Date Dec. 7, 1998 Sec. 102(e) Date Dec. 7, 1998 PCT Filed Jun. 6, 1997 PCT Pub. No. WO97/47605 PCT Pub. Date Dec. 18, 1997The invention relates to a process for the preparation of 4,5,6-trichloro- and 2,4,5,6-tetrachloropyr
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