6,7,8,9-tetrahydro-5h-benzo[7]annulene-2-alkylamine compounds and their uses
A compound, alkylamine technology, applied in the field of medicinal chemistry and drug therapy, can solve the problems of increasing bacterial resistance, increasing bacterial virulence, etc.
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Embodiment 16
[0095] Example 1 Preparation of 6,7,8,9-tetrahydro-5H-benzo[7]rotaxene (Intermediate II)
[0096]
[0097] 1 g of 1-benzocycloheptanone was dissolved in 7.2 ml of trifluoroacetic acid, 1.5 ml of triethylsilane was added, and the mixture was stirred at 60°C overnight. After the reaction was completed, part of the trifluoroacetic acid was removed by rotary evaporation, then the reaction solution was poured into ice water, extracted three times with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, filtered, concentrated, and the residue was subjected to column chromatography The title compound was isolated as 0.91 g of a colorless oil in 90% yield.
[0098] 1 H-NMR (400MHz, CDCl 3 ) δ 7.17-6.96 (m, 4H), 2.79 (dd, J=7.0, 4.1 Hz, 4H), 1.95-1.73 (m, 2H), 1.65 (dd, J=10.0, 4.8 Hz, 4H).
Embodiment 2
[0099] Example 2 Preparation of 2-iodo-6,7,8,9-tetrahydro-5H-benzo[7]rotaxene (Intermediate III)
[0100]
[0101] 675 mg of intermediate II and 1.14 g of N-iodosuccinimide were dissolved in 20 ml of acetic acid, and the reaction was heated at 70° C. for 7 hours under nitrogen protection. After the reaction was completed, the reaction was quenched with an appropriate amount of saturated sodium thiosulfate solution at 0 °C, saturated sodium bicarbonate solution was added, extracted three times with ethyl acetate, washed with saturated brine, dried over anhydrous magnesium sulfate, filtered, concentrated, and the residue The compound was separated by column chromatography to give the title compound, 867 mg as a colorless oil, the yield was 69%.
[0102] 1 H-NMR (400MHz, acetone) δ 7.68 (d, J=6.9Hz, 1H), 7.42 (d, J=7.9Hz, 1H), 6.91 (d, J=7.8Hz, 1H), 2.74 (t, J = 10.2 Hz, 4H), 1.83 (s, 2H), 1.60 (s, 4H).
Embodiment 36
[0103] Example 3 Preparation of 6,7,8,9-tetrahydro-5H-benzo[7]rotaxene-2-carbonitrile (Intermediate IV)
[0104]
[0105]272 mg of intermediate III and 179 mg of cuprous cyanide were added to 10 ml of N,N-dimethylformamide and heated to reflux overnight. After the reaction of intermediate III was completed, it was cooled to room temperature, and concentrated ammonia water was added to the system until the solution became clear, extracted with ethyl acetate three times, washed with saturated brine, dried over anhydrous magnesium sulfate, filtered and concentrated, and the residue was separated by column chromatography. , the title compound was obtained as 122 mg of a pale yellow solid with a yield of 71%.
[0106] 1 H-NMR (400MHz, CDCl 3 )δ7.47-7.28(m, 2H), 7.16(t, J=9.9Hz, 1H), 2.82(t, J=9.4Hz, 4H), 1.86(s, 2H), 1.65(s, 4H).
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