Arylalkylamino-substituted quinazoline analogues
A technology of alkyl and amino groups, applied in the field of probes for detection and localization of capsaicin receptors, can solve the problems of limited therapeutic use, burning pain and the like
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[0299]The mass spectrometry data in this example and the following examples are electrospray MS, and the cone voltage (cone voltage) is 15V or 30V according to the positive ion mode, using the instrument Micromass Time-of-Flight LCT (Micromass, Beverly MA), equipped with Waters 600 pump , Waters 996 photodiode array detector, Gilson 215 autosampler and Gilson 841 microinjector. MassLynx (Advanced Chemistry Development, Inc; Toronto, Canada) version 4.0 software was used. A sample volume of 1 μl was injected into a 50×4.6mm Chromolith SpeedROD C18 column, and a 2-phase linear gradient was used to elute at a flow rate of 6 ml / min. The total absorbance of the sample was measured in the 220-340nm UV range. The dissolution conditions are: mobile phase A-95 / 5 / 0.05 water / MeOH / TFA; mobile phase B-5 / 95 / 0.025 water / MeOH / TFA.
[0300] Gradient: time(minutes) %B
[0301] 0 10
[0302] 0.5 100
[0303] ...
example 1
[0307] Preparation of representative aralkylamino-substituted quinazoline analogs
[0308] This example illustrates representative aralkylamino-substituted quinazoline analogs [4-(2-fluoro-phenyl)-ethyl]-[7-(3-trifluoromethyl-pyridin-2-yl)-quinoline Preparation method of oxazolin-4-yl]-amine (compound I).
[0309]
[0310] Take 4-chloro-7-(3-trifluoromethyl-pyridin-2-yl)-quinazoline (10.8 mg, 35 micromoles) and 2-fluorophenethylamine (5.4 mg, 38.5 micromoles) in 392.5 µl CH 3 CN. DIEA (9.1 μL, 52.5 μmol) was added and the reaction mixture was heated at 45°C overnight. The reaction was cooled to room temperature and washed with 1N NaOH (200 μl). The organic phase was packed into a 0.5 g silica gel SPE column. Impurities were eluted with 4 mL 9 / 1 hexane / EtOAc. The product was collected from the eluate with 4 mL of EtOAc. The solvent was removed in vacuo to give [4-(2-fluoro-phenyl)-ethyl]-[7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]- Amine as a white soli...
example 2
[0312] Synthesis of other representative aralkylamino-substituted quinazoline analogs
[0313] This example illustrates the preparation of other representative substituted 2-aminoalkyl-quinazolin-4-ylamine analogs.
[0314] A. [2-Chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-phenethylamine (compound 4)
[0315]
[0316] 4-Chloro-2-chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazoline (333 mg, 0.93 mmol) was dissolved in 5 mL of acetonitrile at room temperature. DIEA (162 μL, 0.93 μmol) was added followed by phenethylamine (117 μL, 0.93 μmol). The reaction mixture was stirred at room temperature for 3 hours. The solvent was removed in vacuo. The residue is soluble in CH 2 Cl 2 Then pass through a 5 g silica gel SPE column. Unreacted starting material was removed by eluting with 5 mL of dichloromethane. The product is 95 / 5CH 2 Cl 2 / Methanol eluate collection. The solvent was removed in vacuo to give [2-chloromethyl-7-(3-trifluoromethyl-...
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