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A technology of anagrelide hydrochloride and Lewis acid, which is applied in the direction of organic chemistry and the like, can solve the problems of long synthesis route of anagrelide hydrochloride, difficult product purification, high cost per unit consumption, and achieves less impurities, short synthesis route and single cost. low consumption effect
Inactive Publication Date: 2013-08-21
HEILONGJIANG UNIV
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[0014] The present invention aims to solve the technical problems that the existing anagrelide hydrochloride has a relatively long synthetic route, the toxic reagent cuprous cyanide is used in the synthetic route, the product has many impurities, the product is difficult to purify, and the cost per unit consumption is high, thereby providing a hydrochloric acid The preparation method of anagrelide
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specific Embodiment approach 1
[0030] Specific embodiment one: the preparation method of a kind of anagrelide hydrochloride of the present embodiment is carried out according to the following steps:
[0031] 1. Add 2000mL of THF into the three-necked flask, under the protection of nitrogen, add sodium borohydride, Lewis acid and 2,3-dichlorobenzoic acid, stir well at room temperature, add 260-270g of iodine in THF solution dropwise, drop After the addition, heat to reflux for 12-24 hours, then cool to room temperature, add methanol dropwise until the solution is clear, concentrate under reduced pressure, add 2000 mL of KOH solution with a mass concentration of 20%, hydrolyze at 20-60°C for 5-10 hours, and then Extract with a mixed solvent of dichloromethane / ethyl acetate, combine the organic layers, dry, filter, concentrate, and recrystallize from toluene to obtain 2,3-dichlorobenzyl alcohol as a white solid; wherein, 2,3-dichlorobenzoic acid, The mol ratio of sodium borohydride and Lewis acid is 1: (2~3): ...
specific Embodiment approach 2
[0043] Embodiment 2: This embodiment is different from Embodiment 1 in that: in step 1, hydrolyze at 40° C. for 5 hours. Others are the same as in the first embodiment.
specific Embodiment approach 3
[0044] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the Lewis acid in step 1 is aluminum trichloride, tin dichloride, zinc chloride, ferric chloride or boron trifluoride. Others are the same as in the first or second embodiment.
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Abstract
The invention relates to a preparation method of anagrelide hydrochloride, and relates to preparation methods of chemical raw materials. The preparation method provided by the invention mainly solves the technical problems that an existing synthetic line of anagrelide hydrochloride is long, a toxic reagent, namely cuprous cyanide is used in the synthetic line, many impurities exist in the product, the product is hard to purify and the cost and unit consumption are high. The preparation method comprises the following steps: 1, preparing 2, 3-dichlorbenzyl alcohol; 2, preparing 2, 3-dichloro-6-nitrobenzyl alcohol; 3, preparing 2, 3-dichloro-6-nitryl-benzyl chloride; 4, preparing N-(2, 3-dichloro-6-nitrobenzyl) glycine ethyl ester hydrochloride; 5, preparing N-(6-amino-2, 3-dichlorobenzyl) glycine ethyl ester; 6, preparing an anagrelide hydrochloride crude product; and 7, preparing anagrelide hydrochloride. The preparation method provided by the invention is simple in synthetic process, shorter in synthetic line, low in cost and unit consumption, high in yield and less in three wastes generated in the reaction process, and is suitable for industrialized production. The preparation method provided by the invention is applied to the field of preparation of chemical raw materials.
Description
technical field [0001] The invention relates to a method for preparing chemical raw materials. technical background [0002] Platelet aggregation inhibitor Anagrelide is an oral anti-platelet aggregation drug, a cyclic adenosine monophosphate (cMAP) phosphodiesterase (PDE) inhibitor, chemical name 6,7-dichloro-1,2,3,5 -Tetrahydroimidazo-[2,1-b]quinazolin-2-(3H)-one, trade name Agrylin, was developed by Roberts Phnaajeeutieals in the United States, and was approved for listing in the United States in July 1997. The drug has strong selectivity, no serious side effects of leukopenia, anemia and leukemia. It is currently used to treat thrombocytosis caused by essential thrombocythemia and myeloproliferative diseases, and is the first drug approved for essential thrombocythemia. The chemical formula of the substance: [0003] [0004] The synthetic method of anagrelide hydrochloride, bibliographical information mainly contains three kinds: [0005] Method 1 (US4146718) use...
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