STING protein agonist coupled with compound
A compound, optionally a technology, applied in the fields of organic chemistry, antiviral agents, drug combinations, etc., can solve the problems of failure to observe obvious curative effect, failure to activate human STING protein, etc.
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Embodiment 1
[0048] Compound 1
[0049] Compound 1 was prepared by the following steps:
[0050]
[0051] The first step: N-tert-butoxycarbonyl-N'-benzyloxycarbonyl-L-ornithine 1a (25g, 68mmol), triethylamine (11.5mL, 81.9mmol) were dissolved in tetrahydrofuran (100mL), in Isobutyl chloroformate (10mL, 79mmol) was added dropwise in ice bath, stirred for half an hour in ice bath, sodium borohydride (7.8g, 205mmol), water (3mL, slowly added dropwise) were added successively, and the mixture was continued under ice bath Stir for 2 hours. LC-MS monitored the completion of the reaction, added water (150mL) to quench, extracted the aqueous phase (150mL*3) with ethyl acetate, combined the organic phases, dried over anhydrous sodium sulfate, filtered, and concentrated to obtain compound 1b (20g) as a colorless oil Liquid, 83% yield. ESI-MS(m / z):353.6[M+H] + ; 1 H NMR (500MHz, DMSO-d6) δppm 7.39-7.25 (m, 5H), 7.19 (t, J = 5.2Hz, 1H), 6.43 (d, J = 8.3Hz, 1H), 4.98 (s, 2H), 4.53(t,J=5.4Hz,1H...
Embodiment 2
[0067] Compound 2 was prepared by the following steps:
[0068]
[0069] The first step: N-tert-butoxycarbonyl-N'-benzyloxycarbonyl-D-ornithine 2a (25g, 68mmol), triethylamine (11.5mL, 81.9mmol) were dissolved in tetrahydrofuran (100mL), in Isobutyl chloroformate (10mL, 79mmol) was added dropwise in ice bath, stirred for half an hour in ice bath, sodium borohydride (7.8g, 205mmol), water (3mL, slowly added dropwise) were added successively, and the mixture was continued under ice bath Stir for 2 hours. LC-MS monitored the completion of the reaction, quenched with water (150 mL), extracted the aqueous phase (150 mL*3) with ethyl acetate, combined the organic phases, dried over anhydrous sodium sulfate, filtered, and concentrated to obtain compound 2b (22 g), a colorless oil Liquid, 91% yield. ESI-MS(m / z):353.6[M+H] + .
[0070] Step 2: Dissolve compound 2b (22g, 56mmol) in dichloromethane (200mL), add hydrogen chloride-1,4-dioxane solution (4N, 75mL, 300mmol), and stir o...
Embodiment 3
[0083] Compound 3 was prepared by the following steps:
[0084]
[0085] Step 1: Dissolve compound 2j (200mg, 0.48mmol) in N,N-dimethylformamide (4mL), and add compound 3a (200mg, 1mmol) and cesium carbonate (326mg, 1mmol) sequentially. The reaction mixture was stirred overnight at 70°C. After the reaction was monitored by LC-MS, water (20 mL) was added, and the aqueous phase (50 mL*3) was extracted with ethyl acetate. The organic phase was combined and separated by silica gel column chromatography to obtain compound 3b (235 mg ), white solid, yield 84%. ESI-MS(m / z):576.6[M+H] + .
[0086] The second step: compound 3b (235 mg, 0.4 mmol) was dissolved in methanol (20 mL), and ammonia water (8 mL) was added. Then sodium dithionite (350 mg, 2 mmol) was dissolved in water (6 mL), and the reaction solution was slowly added at room temperature, and the stirring was continued for half an hour. LC-MS monitored the completion of the reaction, added water (50 mL), extracted the a...
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