Resorcinol formaldehyde derivative containing substituted biphenyl and application thereof
A technology of resorcinol methyl ether and derivatives, applied in drug combination, nitrile/isonitrile active ingredients, organic chemistry, etc., can solve the problem of unsatisfactory PD-1/PD-L1 inhibitory effect
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Embodiment 1
[0046] Embodiment 1 (preparation C1)
[0047] The structural formula is The preparation method of the compound consists of the following steps:
[0048] Step 1: Preparation of Compound V
[0049]
[0050] 4g 5-chloro-2,4-dihydroxybenzaldehyde (compound VII) and 5g (3-(2,3-dihydrobenzo[b][1,4]dioxan-6-yl)- 2-methylphenyl)methanol (compound VI), 8.4g triphenylphosphine (PPh 3 ) was added in 50ml of anhydrous tetrahydrofuran, stirred for 15 minutes, 8.2mL of diisopropyl azodicarboxylate (DIAD) was dripped into the reaction solution in small quantities in batches, reacted for 10 hours, monitored by thin layer chromatography (TLC), and the reaction ended Afterwards, the reaction solution was poured into 100mL water, extracted with ethyl acetate (100mL×5), allowed to stand for liquid separation, and the organic phase was washed with 5% sodium bicarbonate (NaHCO 3 ) (80mL×3), washed with saturated brine (80mL×3), then dried with anhydrous magnesium sulfate, filtered with suct...
Embodiment 2
[0062] Embodiment 2 (preparation C2)
[0063] The structural formula is The preparation method of the compound consists of the following steps:
[0064] Step 1: Preparation of C2
[0065]
[0066]Add 40mg of compound III and 50mg of (R)-pyrrolidine-3-carboxylic acid, 2 drops of glacial acetic acid into 5ml of anhydrous methanol, stir, heat to 60°C, react for 4 hours, then add 40mg of sodium cyanoborohydride (NaBH 3 CN), reacted at room temperature for 12 hours, monitored by TLC, after the reaction was completed, the solvent was spin-dried, and the reactant was poured into 100mL water, extracted with ethyl acetate (20mL×3), left to separate liquids, and the organic phase was respectively washed with 5% NaHCO 3 (20mL×3), washed with saturated brine (20mL×3), then dried over anhydrous magnesium sulfate, filtered with suction, removed ethyl acetate under reduced pressure, and then performed column chromatography V (dichloromethane): V (methanol) =20:1 yielded 6 mg of whit...
Embodiment 3
[0069] Embodiment 3 (preparation C3)
[0070] The structural formula is The preparation method of the compound consists of the following steps:
[0071] Step 1: Preparation of C3
[0072]
[0073] Add 40mg of compound III and 55mg (R)-3-pyrrolidinol, 2 drops of glacial acetic acid into 5ml of anhydrous methanol, stir, heat to 60°C, react for 4 hours, then add 50mg of sodium cyanoborohydride (NaBH 3 CN), reacted at room temperature for 12 hours, monitored by TLC, after the reaction was completed, the solvent was spin-dried, and the reactant was poured into 100mL water, extracted with ethyl acetate (20mL×3), left to separate liquids, and the organic phase was respectively washed with 5% NaHCO 3 (20mL×3), washed with saturated brine (20mL×3), then dried over anhydrous magnesium sulfate, filtered with suction, removed ethyl acetate under reduced pressure, and then performed column chromatography V (dichloromethane): V (methanol) =20:1 yielded 4 mg of white solid compound ...
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