Crystalline Anti-trichophyton agents and preparation process thereof
A technology of crystallization and compounding, applied in antibacterial drugs, antifungal agents, pharmaceutical formulations, etc., can solve undisclosed problems and achieve high stability, easy storage and handling
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0088] Example 1: Preparation of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenol
[0089]1) Add 390 mL of dehydrated tetrahydrofuran to 25.6 g of 3,5-dimethyl-1-(4-methylphenyl)-1H-pyrazole, and cool to -5 to 0°C under a nitrogen atmosphere. 78 mL (1.5 equivalents) of a 2.65 M n-butyllithium n-hexane solution was added dropwise, and stirred at -5 to 0°C for 1 hour. 64 mL (2.0 equivalents) of triisopropyl borate was added, and stirred at 0-10° C. for 30 minutes. 390 mL of 10% ammonium chloride solution was added, and the pH was adjusted to 4.5 with 6M hydrochloric acid, followed by extraction with 390 mL of ethyl acetate, and the aqueous layer was removed. After washing the organic layer with 240 mL of 15% brine, the organic layer was concentrated to 120 mL under reduced pressure. Add 240 mL of acetone and concentrate to 120 mL under reduced pressure to obtain the acetone of 2-{(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenyl}boronic acid (formula (6)). solution.
[0090] 2-{(...
Embodiment 2
[0097] Example 2: Preparation of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenol
[0098] 7 mL of dehydrated tetrahydrofuran was added to 278.8 mg of 3,5-dimethyl-1-(4-methylphenyl)-1H-pyrazole, and cooled to 0°C under a nitrogen atmosphere. 1 mL (1.1 equivalent) of a 1.64 M n-butyllithium n-hexane solution was added dropwise, and stirred at 0° C. for 30 minutes. 0.5 mL (1.5 equivalents) of triisopropyl borate was added, and stirred at 0° C. for 1 hour. 7 mL of water and 20 mL of toluene were added thereto, and the pH was adjusted to 1.0 with 1M hydrochloric acid, followed by stirring at room temperature for 30 minutes. Adjust pH = 4 with 1M sodium hydroxide solution and remove the aqueous layer. After washing the organic layer with 10 mL of 15% brine, the organic layer was concentrated under reduced pressure to obtain 2-{(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenyl } Boric acid 318mg.
[0099] 5 mL of acetone was added to this 2-{(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphe...
Embodiment 3
[0101] Example 3: Preparation of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenol
[0102] 40 mL of dehydrated tetrahydrofuran was added to 2.65 g of 3,5-dimethyl-1-(4-methylphenyl)-1H-pyrazole, and cooled to 0° C. under a nitrogen atmosphere. 13.0 mL (1.5 equivalents) of a 1.64 M n-butyllithium n-hexane solution was added dropwise, and stirred at 0° C. for 30 minutes. 6.6 mL (2.0 equivalents) of triisopropyl borate was added, followed by stirring at 0° C. for 1 hour. 40 mL of 10% ammonium chloride solution was added, the pH was adjusted to 4 with 2M hydrochloric acid, extraction was performed with 53 mL of ethyl acetate, and the aqueous layer was removed. After washing the organic layer with 27 mL of 15% saline, the organic layer was concentrated under reduced pressure to obtain 2-{(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenyl } Boric acid 3.45g.
[0103] 48 mL of acetone was added to this 2-{(3,5-dimethyl-1H-pyrazol-1-yl)-5-methylphenyl}boronic acid, and cooled to 0-5°C. 4...
PUM
| Property | Measurement | Unit |
|---|---|---|
| diffraction angle | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More