2,3-dihydro-1h-indene-2-ylurea derivative and pharmaceutical application of same
A technology of derivatives and urea, applied in the field of 2,3-dihydro-1H-inden-2-ylurea derivatives and their pharmaceutical applications, can solve the problems of QOL reduction and intractability
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Embodiment 1
[0248] 1-(5-tert-butyl-3-(hydroxymethyl)-2-methoxyphenyl)-3-((1S,2R)-1-hydroxy-2,3-dihydro-1H-indene- Synthesis of 2-yl)urea (compound 1)
[0249]
[0250] 〔the first process〕
[0251] Synthesis of 5-tert-butyl-2-methoxy-3-nitrobenzaldehyde
[0252] A solution of 5-tert-butyl-2-hydroxybenzaldehyde (7.71 g, 43.3 mmol) in acetonitrile (216 mL) was cooled to -40°C, and nitronium tetrafluoroborate (7.47 g, 56.2 mmol) was added. The temperature was raised to -20°C over 1 hour while stirring. Water was added to the reaction liquid, and the aqueous layer was extracted with ethyl acetate. The organic layer was washed with saturated brine. The organic layer was dried over anhydrous sodium sulfate, filtered, and the solvent was distilled off under reduced pressure. To a DMF (50.0 mL) suspension of the obtained residue (8.35 g) and potassium carbonate (25.9 g, 187 mmol) was added iodomethane (8.19 mL, 131 mmol), followed by stirring at room temperature for 15 hours. Water was ad...
Embodiment 2
[0266] 1-(5-tert-butyl-3-(hydroxymethyl)-2-methoxyphenyl)-3-((1S,2R)-4-fluoro-1-hydroxy-2,3-dihydro- Synthesis of 1H-inden-2-yl)urea (Compound 3)
[0267]
[0268] Using 2,2,2-trichloroethyl 5-tert-butyl-3-(hydroxymethyl)-2-methoxyphenylcarbamate (0.100 g, 0.260 mmol) and (1S, 2R)- 2-Amino-4-fluoro-2,3-dihydro-1H-inden-1-ol·L-tartrate (0.091g, 0.286mmol), by carrying out the same reaction as in Example 1 [fifth step], 0.034 g of the title compound was obtained (yield 32%).
Embodiment 3
[0270]1-(5-tert-butyl-2-methoxy-3-((S)-2,2,2-trifluoro-1-hydroxyethyl)phenyl)-3-((1S,2R)- 1-hydroxy-2,3-dihydro-1H-inden-2-yl)urea (compound 46a), 1-(5-tert-butyl-2-methoxy-3-((R)-2,2 , 2-trifluoro-1-hydroxyethyl)phenyl)-3-((1S,2R)-1-hydroxyl-2,3-dihydro-1H-inden-2-yl)urea (compound 46b) synthesis
[0271]
[0272] 〔the first process〕
[0273] Synthesis of 1-(5-tert-butyl-2-methoxy-3-nitrophenyl)-2,2,2-trifluoroethanol
[0274] The solution of 5-tert-butyl-2-methoxy-3-nitrobenzaldehyde (13.5g, 57.1mmol) in THF (57.1mL) was cooled to 0°C, and trimethyl (trifluoromethyl) was added dropwise Silane (10.9 mL, 74.2 mmol), 1.0 mol / L tetra-n-butylammonium fluoride / THF solution (5.71 mL, 5.71 mmol). After adding the reagents, the temperature was raised to room temperature. After stirring for 3 hours, 1 mol / L hydrochloric acid was added to the reaction liquid, and stirred at room temperature for 2 hours. The aqueous layer was extracted with ethyl acetate, and the organic layer ...
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