A kind of compound and preparation method and application
A compound and mixture technology, applied in the field of chemistry, can solve the problem of influenza virus easily producing drug-resistant strains, etc., and achieve the effects of high safety index, simple preparation method, and easy availability of raw materials
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Embodiment 1
[0296] The synthesis of embodiment 1 intermediate Ia'-i'
[0297] Weigh 2.00g (13.3mmol) of p-tolueneacetic acid in a 50ml round bottom flask, add 10ml of tetrahydrofuran (THF) to dissolve completely, then add 1.956g (16mmol) of ethyl chloroacetate and 1.624g (16mmol) of triethylamine , Heating to reflux at 60°C for 6.5h. TLC spots the plate to monitor the completion of the reaction, and cools to room temperature. The triethylamine salt generated in the reaction was removed by suction filtration, the filter cake was washed three times with THF, and concentrated under reduced pressure to obtain a light yellow transparent liquid. (3×15) extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, concentrated by suction filtration to obtain intermediate Ie'.
[0298] The structural formula of intermediate Ie' described in the present embodiment is Molecular formula is C 13 h 16 o 4 .
[0299] In the above method, p-methylphenylacetic ac...
Embodiment 2
[0307] The synthesis of embodiment 2 intermediate IIa-i
[0308] Taking IIe as an example, weigh 3.50g (18.3mmol) of the intermediate I (Ia'-i') prepared in Example 1 in a 50ml round bottom flask, and add 15ml of N,N-dimethylformamide ( DMF) was dissolved, stirred under ice-bath conditions, and potassium tert-butoxide was added in 6 times within 30 min, a total of 3.42 g (36.6 mmol). The reaction was stirred for 30 min in an ice bath, and then stirred for 3 h at room temperature. TLC monitors that the reaction is complete. Add 20ml of water to dilute the reaction system, and then adjust the pH to 2-3 with 5wt% dilute HCl under ice bath conditions. During the pH adjustment process, a light yellow solid is continuously precipitated in the system. Water was then slowly added to the system until no obvious solid precipitated out (100ml of water). Place in the refrigerator overnight, filter with suction, and wash the filter cake three times with water (3*10ml) to obtain a pale ye...
Embodiment 3
[0312] The synthesis of embodiment 3 intermediate III-1a-i
[0313] Taking III-1e as an example, weigh 1.50g (7.88mmol) of intermediate II (obtained in Example 2) in a 50ml round bottom flask, add 15ml of acetone to dissolve completely, and add 1.525g (11.1mmol) of anhydrous potassium carbonate. Dissolve 1.193 g (9.5 mmol) of dimethyl sulfate in 10 ml of acetone, and slowly add it dropwise into the reaction system through a constant pressure dropping funnel, and the dropwise addition is completed within 30 minutes. Under the condition of avoiding light at room temperature, the reaction was carried out for 10 h. The reaction was complete as monitored by TLC, and the reaction solvent was removed by concentration under reduced pressure. After adding 25 ml of water, anhydrous potassium carbonate was dissolved, and a large amount of light yellow solid was precipitated at the same time. Suction filtration, the filter cake was washed three times with water (3 × 10 ml) to obtain a li...
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