A common heterocyclic compound, 35180-01-9, name is Chloromethyl isopropyl carbonate, molecular formula is C5H9ClO3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. 35180-01-9.
S03 condensation: After pretreating the crude tenofovir obtained in the step S02, and stirring 16 L of N-methylpyrrolidone and 4.44 kg of triethylamine, the temperature is raised to 50 C and stirred.11.15 kg of isopropyl chloromethyl carbonate was added dropwise, stirred, and the reaction was completely cooled and quenched.After cooling, add 12 L of cyclohexane twice, stir, centrifuge, layer, and discard the upper layer of cyclohexane. The lower layer of the filtrate was transferred to a reaction kettle, and 30 L of water and 20 L of ethyl acetate were added.After stirring for 30 minutes, the layers were allowed to stand, and the aqueous layer was extracted with 10 L of ethyl acetate.Wash with 20L of 10wt% brine, add 1.0kg anhydrous sodium sulfate, stir dry, centrifuge,The filtrate is transferred to the transfer reactor in batches, concentrated under reduced pressure, and the concentrate is transferred to the reaction vessel.Denotefovir dipivoxilCrude.
The synthetic route of Chloromethyl isopropyl carbonate has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shandong Kexing Biological Products Co., Ltd.; Hao Zhihai; Wang Cuicui; Lu Fuxin; Guo Chao; Wang Jun; Zhang Yun; Qiu Duxian; Cui Ning; (26 pag.)CN108409789; (2018); A;,
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