Benzo[5,6]cycloheptyl[1,2-b]pyridine derivative, preparation method, pharmaceutical composition and use thereof for anti-allergic diseases
A technology of compounds and alkyl groups, applied in allergic diseases, drug combinations, antipyretics, etc.
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Embodiment 1
[0048] 8-Chloro-11-{1-[(5-phenyl-2-[1,3,4]oxadiazolyl)methyl]4-piperidinylidene}-6,11-dihydro-5H- Benzo[5,6]cycloheptane[1,2-b]pyridine (I 1 )
[0049] 1. Preparation of methyl benzoate
[0050] Weigh 3 g of benzoic acid dissolved in 15 ml of methanol, then add 15 ml of cyclohexane, then slowly add concentrated H 2 SO 4 1ml, reflux for 7h, and use a water separator to separate the water generated by the reaction during the reflux. After the reaction is over, the reaction solution is concentrated under reduced pressure to about 1 / 3 volume, poured into water, and diluted with 1% NaHCO 3 The solution adjusted the mixture to neutral, and extracted with ethyl acetate, 10 ml each time, until the ethyl acetate layer had no fluorescence under the ultraviolet lamp. The ethyl acetate layers were combined and backwashed once with saturated NaCl solution, and then washed with anhydrous NaCl 2 SO 4 After drying, the ethyl acetate was evaporated to dryness to obtain 3.33 g of a color...
Embodiment 2
[0063] 8-Chloro-11-{1-[(5-(2-n-butoxyphenyl)-2-[1,3,4]oxadiazolyl)methyl]4-piperidinylidene}-6 , 11-dihydro-5H-benzo[5,6]cycloheptane[1,2-b]pyridine (I 2 )
[0064] 1. Preparation of Methylparaben
[0065] Using p-hydroxybenzoic acid as raw material, the preparation method is the same as that of methyl benzoate, white crystal, mp: 165-167°C, yield 98.7%.
[0066] 2. Preparation of methyl 4-n-butoxybenzoate
[0067] Dissolve 3g of methyl p-hydroxybenzoate in 30ml of ethyl acetate, add K 2 CO 3 2.6g, then add 4ml of n-bromobutane dropwise, heat to reflux for 8h, end the reaction, filter out the remaining solid and wash the solid with ethyl acetate until the lotion does not show fluorescence under the ultraviolet lamp. Combine the filtrate and washing liquid, mix the sample with crude silica gel, make sand, and separate the product by column chromatography (petroleum ether: ethyl acetate = 10:1) to obtain a colorless transparent oily liquid.
[0068] 3.I 2 preparation of ...
Embodiment 3
[0074] 8-chloro-11-{1-[(5-(2-methoxyphenyl)-2-[1,3,4]oxadiazolyl)methyl]4-piperidinylidene}-6, 11-Dihydro-5H-benzo[5,6]cycloheptane[1,2-b]pyridine (I 3 )
[0075] Preparation method is the same as I 1 . Pale red solid, mp: 154-155°C, yield 78%.
[0076] MS (ESI, 70ev, m / z): 499.2 [M+H] + ;521.2[M+Na] +
[0077] 1 H NMR (300MHz, CDCl 3 ) δ: 2.35-2.58 (m, 6H, = C (CH 2 ) 2 , N(CH 2 ) 2 ); 2.75-2.83(m, 2H, N(CH 2 ) 2 ); 2.88-2.91 (m, 2H, PhCH 2 ); 3.32-3.37(m, 2H, ); 3.92(m, 5H, -OCH 3 ); 7.02-7.13 (m, 6H, Ar); 7.39-7.42 (dd, 1H, ); 7.45-7.51 (m, 1H, Ar); 7.88-7.91 (dd, 1H, Ar); 8.37-8.39 (dd, 1H, )
[0078]IR (cm -1 ): 3357, 2939, 2901, 2823, 1708, 1588, 1477, 1436, 1258, 1243, 1116, 1018, 983, 829, 750
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