Sulfonamides as cccDNA inhibitors
A compound and selected technology, applied in the direction of amide active ingredients, organic chemistry, antiviral agents, etc., can solve the problems of inability to clear and easy to recur.
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reference example 1
[0250] Reference Example 1: Synthesis of Compound BB-1
[0251]
[0252] synthetic route:
[0253]
[0254] Compound BB-1-1 (2.00g) was dissolved in pyridine (20.00mL), then compound BB-1-2 (2.16g) was added at 0°C, and the reaction solution was stirred at 0°C for 5 hours. The reaction was quenched with 2N hydrochloric acid at 0°C. The reaction solution was extracted with ethyl acetate (20 mL*3), the organic phases were combined, washed with brine (20 mL*2), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain a crude product. The crude product was subjected to flash preparative chromatography (petroleum ether: ethyl acetate = 20:1) to obtain the target compound BB-1 (yellow solid, 900 mg). MS (ESI) m / z: 392 [M+Na] + .
reference example 2
[0255] Reference Example 2: Synthesis of Compound BB-2
[0256]
[0257] synthetic route:
[0258]
[0259] Compound BB-2-1 (1.00g) and compound BB-2-2 (1.81g) were dissolved in N,N-dimethylformamide (50.00mL), and HATU (4.83g) was dissolved at 25°C and N,N-diisopropylethylamine (3.28 g) were added to the above reaction liquid, and stirred at 25° C. for 14 hours. The crude product was purified by flash chromatography (petroleum ether: ethyl acetate = 1:1) to obtain the target compound BB-2 (colorless oily liquid, 1.40 g). MS (ESI) m / z: 259 [M+H-tBu] + .
reference example 3
[0260] Reference Example 3: Synthesis of Compound BB-3
[0261]
[0262] synthetic route:
[0263]
[0264] Step 1: Synthesis of Compound BB-3-3
[0265] Compound BB-3-1 (1.00 g) was dissolved in dichloromethane (15.00 mL), and compound BB-3-2 (465.64 mg) was added, and the reaction solution was reacted at 15° C. for 1 hour. The reaction solution was concentrated to obtain a crude product. The crude product was dissolved in 15 mL of dichloromethane and separated by flash preparative chromatography (dichloromethane:methanol=gradient elution, from 1:0 to 10:1) to obtain the target compound BB-3-3 (white solid, 1.50 g). MS (ESI) m / z: 298 [M+H] + .
[0266] Step 2: Synthesis of Compound BB-3
[0267] Compound BB-3-3 (1.50 g) was dissolved in dichloromethane (5.00 mL), and hydrochloric acid in dioxane (4 mol / L, 5.62 mL) was added, and the mixture was reacted at 15° C. for 1.5 hours. The reaction solution was concentrated to obtain the target compound BB-3 (light yellow ...
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