Novel compound and pharmaceutically-acceptable salt thereof
A technology of pharmacology and compounds, applied in the fields of active ingredients of heterocyclic compounds, organic chemistry, antitumor drugs, etc.
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[1032] Hereinafter, although an Example demonstrates this invention in more detail, this invention is not limited to these Examples. In addition, the production methods of the raw material compounds used in the examples are described as reference examples, but these are also illustrations for concretely explaining the implementation of the present invention, and the scope of the present invention is not limited by these examples, and will not be limited by these examples. It is obvious that various applications, modifications, corrections, etc. can be made within the scope of the present invention.
[1033] Hereinafter, the abbreviations in Examples and Reference Examples have the following meanings.
[1034] M: mol / L
[1035] DMSO: dimethyl sulfoxide
[1036] DMPU: N,N'-dimethylpropylene urea
[1037] ESI: Electrospray Ionization
[1038] ee: enantiomeric excess
[1039] HPLC: High Performance Liquid Chromatography
[1040] mCPBA: m-chloroperbenzoic acid
[1041] MS: m...
reference example 1
[1049] 7-Bromo-5-isopropylbenzo[d]oxazole-2-thiol
[1050] (a) 2-Bromo-4-isopropyl-6-nitrophenol
[1051]Dissolve 2.5 g of 2-bromo-4-isopropylphenol in dichloromethane (50 mL), add concentrated sulfuric acid (0.8 mL, 1.3 equivalents) dropwise at 0° C. over 5 minutes, and then add 70% nitric acid (0.7 mL , 1.0 equivalent) was added over 5 minutes, and stirred at room temperature for 2 hours. After confirming the product by TLC, the pH was adjusted to 7 by adding solid sodium bicarbonate. The reaction solution was filtered, the filtrate was extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate. This was filtered, and the filtrate was concentrated under reduced pressure to obtain 2.8 g of the resulting title compound as a crude product.
[1052] MS (ESI) m / z: 260 (M-H) -
[1053] (b) 2-Amino-6-bromo-4-isopropylphenol
[1054] Sodium dithionite (9.4 g, 5 equivalents) was dissolved in distilled water (32 mL) at 0° C., and 2.8 g of 2-br...
reference example 2
[1059] 7-Bromo-4-methylbenzo[d]oxazole-2-thiol
[1060] (a) 6-bromo-3-methyl-2-nitrophenol
[1061] The title compound was obtained from 2.5 g of 2-bromo-5-methylphenol in the same manner as in Reference Example 1(a) except that the crude product was purified by silica gel column chromatography (hexane:ethyl acetate=95:5). 1.5g.
[1062] MS (ESI) m / z: 230 (M-H) -
[1063] (b) 2-Amino-6-bromo-3-methylphenol
[1064] Using the same method as in Reference Example 1(b), 610 mg of the title compound was obtained from 1.5 g of 6-bromo-3-methyl-2-nitrophenol obtained in Reference Example 2(a).
[1065] MS (ESI) m / z: 200 (M-H) -
[1066] (c) 7-bromo-4-methylbenzo[d]oxazole-2-thiol
[1067] Using the same method as in Reference Example 1(c), 360 mg of the title compound was obtained from 610 mg of 2-amino-6-bromo-3-methylphenol obtained in Reference Example 2(b).
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