Method for preparing baloxavir intermediate and intermediate obtained by method
A technology for intermediates and compounds, applied in the field of pharmaceutical synthesis, can solve the problems of unsuitability for industrial production, irritating odor of thiophenol, high toxicity and the like
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Embodiment 1
[0043] Synthesis of Compound A-1
[0044]
[0045] Add 3,4-difluorobromobenzene (20g) and tetrahydrofuran (40ml) into the reaction flask, under the protection of nitrogen, control the internal temperature below -50°C, drop lithium diisopropylamide (LDA, 62ml, 2mol / L tetrahydrofuran solution), the dropwise addition is completed, the internal temperature is controlled below -50°C, and the reaction is carried out for 1 hour, then the temperature is controlled below -20°C, and dimethyl sulfate (15.6g) is added dropwise, after the dropwise addition is completed, the temperature is naturally raised and stirred React for 1 to 2 hours. After the reaction was completed by the central control monitoring, post-processing steps such as quenching and extraction were carried out, and most of the solvent was removed by rotary evaporation to obtain the crude product of compound A-1 (containing part of the solvent). The H NMR spectrum of compound A-1 is shown in figure 1 .
[0046] Synt...
Embodiment 2
[0062]
[0063] Under nitrogen protection, the temperature was controlled below -70°C, dry methyl tert-butyl ether and LDA (40mmol) were added to the reaction flask, the temperature was controlled below -60°C, and the raw material (30mmol) of formazan was added dropwise. Base tert-butyl ether solution; keep the temperature at -40°C, add iodomethane (42mmol), the reaction system immediately produces a yellow solid, and the reaction is exothermic violently. After the addition, the temperature of the system was raised to room temperature, and the reaction solution turned yellow with a large amount of solids. The reaction was carried out at room temperature for 3 hours, and the reaction was stopped by monitoring in the central control system. After post-processing, 13.5 g of the crude product of A-1 was obtained.
[0064] Synthesis of Compound A-2
[0065]
[0066] Add compound A-1 (482g) and tetrahydrofuran (250ml) into the reaction flask, protect it with nitrogen, control ...
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