Pharmaceutical product comprising a muscarinic receptor antagonist and a beta2-adrenoceptor agonist
A technology of receptor agonists and pharmaceutical products, applied in the direction of medical preparations containing active ingredients, drug combinations, pharmaceutical formulations, etc., can solve problems such as unsatisfactory drug efficacy
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[0164] Preparation of muscarinic antagonist
[0165] The muscarinic antagonist of the present invention can be prepared as follows. Alternative salts of those described in this application can be prepared by conventional chemical action using methods similar to those described.
[0166] General experimental details for dry preparation of muscarinic antagonists
[0167] Unless otherwise specified, the following general conditions are used in the preparation of muscarinic antagonists.
[0168] Unless otherwise specified, all reactions were performed under a nitrogen atmosphere.
[0169] In the embodiment, the NMR spectrum is measured on a Varian Unity Inova spectrometer with a proton frequency of 300 or 400 or 500MHz, or on a Bruker DRX spectrometer with a proton frequency of 400 or 500MHz, or on a BrukerAvance spectrometer with a proton frequency of 600MHz The frequency is measured, or on a Bruker Avance DPX 300 spectrometer at a proton frequency of 300MHz. The MS spectrum was measur...
Example Embodiment
[0199] Example 1: (R)-3-(1-Phenyl-cycloheptanecarbonyloxy)-1-(pyrazin-2-ylcarbamoylmethyl)-1-nitrogen -Bicyclo[2.2.2]octane bromide
[0200] a) 1-Phenyl-cycloheptanol
[0201]
[0202] To a solution of magnesium (1.2 g) in anhydrous tetrahydrofuran (60 mL), crystals of iodine were added to a solution of magnesium (1.2 g) in anhydrous tetrahydrofuran (60 mL) under a nitrogen atmosphere at a rate at which the reaction maintained stable reflux, followed by bromobenzene (7.85 g). The reaction mixture was stirred for 20 minutes and then cycloheptanone (4.48 g) was carefully added. After stirring for 10 minutes, saturated aqueous ammonium chloride (10 mL) was added and the reaction mixture was partitioned between water (100 mL) and isohexane (100 mL). Dry the organic layer (MgSO 4 ) And evaporation to give the subtitle compound (7.6g) as an oil.
[0203] 1 H NMR(299.946MHz, CDCl 3 )δ7.53-7.47 (m, 2H), 7.36-7.29 (m, 2H), 7.26-7.19 (m, 1H), 2.07 (ddd, 2H), 1.97-1.50 (m, 11H).
[0204] b) 1...
Example
[0230] For Example 1: (R)-3-(1-phenyl-cycloheptanecarbonyloxy)-1-(pyrazin-2-ylcarbamoylmethyl)-1-nitrogen -Analysis of Bicyclo[2.2.2]octane Bromide Form A
[0231] The sample of crystal form A of Example 1 obtained by the above operation was analyzed by XRPD (PANalytical X'Pert or CubiX system), DSC and TGA.
[0232] The melting temperature of the bromide crystal form A of Example 1 determined by DSC was actually 202°C (initial) (±2°C). The weight loss observed by TGA before melting was 2.7%. GVS determined to obtain a 3% weight gain (%w / w) (±0.2%) at 80%RH.
[0233] Example 1 The XRPD spectrum of bromide crystal form A is in figure 1 Show in.
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