Arylphosphine oxide and arylphosphine sulfide compounds, and preparation method and application thereof
A technology of aryl phosphorus oxides and compounds, applied in the field of medicine, can solve the problem of less HIF-2a inhibitors, and achieve the effect of strong in vitro binding ability
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Embodiment 1
[0031] 3-[7-(dimethylphosphoryl)-2,2-difluoro-1-hydroxyl-2,3-dihydro-1H-indan-4-yl]oxygen-5-fluorobenzonitrile ( Compound 1) synthesis, the structural formula of the compound 1 is as follows:
[0032]
[0033] The preparation method of the compound 1 comprises the following steps:
[0034] (1a): Preparation of 4-methoxy-1-indanone
[0035]
[0036] 4-Hydroxy-1-indanone (2.00g, 13.5mmol) and potassium carbonate (7.5g, 54.0mmol) were added to acetone (40mL), methyl iodide (3.8g, 27.0mmol) was added, the temperature was raised to 60°C, Stir for 5h. TLC showed that the reaction was complete, cooled to room temperature, poured the reaction mixture into water, added ethyl acetate to extract twice, washed the organic phase with brine, dried over anhydrous sodium sulfate, and concentrated to dryness to obtain 4-methoxy- 1-Indanone (2.18 g, 99% yield).
[0037] LCMS (ESI): m / z: 163.1 [M+1].
[0038] (1b): Preparation of 7-iodo-4-methoxy-indan-1-one
[0039]
[0040] To a...
Embodiment 2
[0074] 3-[(1S)-7-(dimethylphosphoryl)-2,2-difluoro-1-hydroxy-2,3-dihydro-1H-indan-4-yl]oxy-5-fluoro Benzonitrile (Compound 2)
[0075]
[0076] At 0°C, RuCl(p-isopropyltoluene)[(R,R)-Ts-DPEN] (16 mg, 0.025 mmol) was added to nitrogen-flushed 3-[(7-(dimethylphosphoryl)- 2,2-Difluoro-1-oxo-indan-4-yl)oxy]-5-fluoro-benzonitrile (150mg, 0.40mmol), formic acid (80mg, 1.58mmol) and triethylamine (0.15 mL, 1.0 mmol) in dichloromethane (20 mL). The vial was sealed and placed in a 4°C refrigerator overnight. TLC showed that the reaction was complete, the reaction mixture was spin-dried and the residue was purified by column chromatography (dichloromethane:methanol=40:1) to obtain 3-[(1S)-7-(dimethylphosphoryl)-2 , 2-Difluoro-1-hydroxy-2,3-dihydro-1H-indan-4-yl]oxy-5-fluorobenzonitrile (120 mg, 80%).
[0077] 1 H NMR (500MHz, DMSO-d 6 ): δ7.72(m, 2H), 7.68(d, J=4Hz, 1H), 7.45(dd, J=12Hz, 1H), 7.10(d, J=8Hz, 1H), 6.76(d, J= 8 Hz, 1H), 5.45 (m, 1H), 3.40 (m, 2H), 1.77 (t, 6H). L...
Embodiment 3
[0079] 3-[(1R)-7-(dimethylphosphoryl)-2,2-difluoro-1-hydroxy-2,3-dihydro-1H-indan-4-yl]oxy-5-fluoro Benzonitrile (compound 3)
[0080]
[0081] At 0°C, RuCl(p-isopropyltoluene)[(S,S)-Ts-DPEN] (16 mg, 0.025 mmol) was added to nitrogen-flushed 3-[(7-(dimethylphosphoryl)- 2,2-Difluoro-1-oxo-indan-4-yl)oxy]-5-fluoro-benzonitrile (150mg, 0.40mmol), formic acid (80mg, 1.58mmol) and triethylamine (0.15 mL, 1.0 mmol) in dichloromethane (20 mL). The vial was sealed and placed in a 4°C refrigerator overnight. TLC showed that the reaction was complete, the reaction mixture was spin-dried and the residue was purified by column chromatography (dichloromethane:methanol=40:1) to obtain 3-[(1R)-7-(dimethylphosphoryl)-2 , 2-Difluoro-1-hydroxy-2,3-dihydro-1H-indan-4-yl]oxy-5-fluorobenzonitrile (122 mg, 81%).
[0082] 1 H NMR (500MHz, DMSO-d 6 ): δ7.71(m, 2H), 7.68(d, J=4Hz, 1H), 7.45(dd, J=12Hz, 1H), 7.10(d, J=8Hz, 1H), 6.76(d, J= 8 Hz, 1H), 5.44 (m, 1H), 3.40 (m, 2H), 1.77 (t, 6H). L...
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