Application of composition of diethylamino and piperazinyl derivatives of Harrisotone A in anti-rhinitis medicine
A technology of composition and rhinitis, applied in the direction of drug combination, medical preparations containing active ingredients, pharmaceutical formulas, etc., can solve the problems of ineffectiveness and poor curative effect of rhinitis
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0011] The preparation of embodiment 1 compound Harrisotone A
[0012] The preparation method of compound Harrisotone A (I) refers to the literature published by Sheng Yin et al. (Sheng Yin et al., 2009.Harrisotones A–E, five novel prenylated polyketides with a rarespirocyclic skeleton from Harrisonia perforata.Tetrahedron 65(2009) 1147–1152 )Methods.
[0013]
Embodiment 2
[0014] The synthesis of the O-bromoethyl derivative (II) of embodiment 2 Harrisotone A
[0015] Compound I (472 mg, 1.00 mmol) was dissolved in 15 mL of benzene, and tetrabutylammonium bromide (TBAB) (0.08 g), 1,2-dibromoethane (3.760 g, 20.00 mmol) and 6 mL of 50% sodium hydroxide solution. The mixture was stirred at 35 °C for 3 h. After 3h, the reaction solution was poured into ice water, extracted twice with dichloromethane immediately, and the organic phase solutions were combined. Then the organic phase solution was washed twice with water and saturated brine successively, then dried with anhydrous sodium sulfate, and finally concentrated under reduced pressure to remove the solvent to obtain a crude product. The crude product was purified by silica gel column chromatography (mobile phase: petroleum ether / acetone=100:1.5, v / v), the brown concentrated elution band was collected and the solvent was evaporated to obtain a yellow powder of compound II (602mg, 76%) .
[00...
Embodiment 3
[0019] The synthesis of the O-(diethylamino) ethyl derivative (III) of embodiment 3 Harrisotone A
[0020] Compound II (396mg, 0.5mmol) was dissolved in 15mL of acetonitrile, anhydrous potassium carbonate (345mg, 2.5mmol), potassium iodide (84mg, 0.5mmol) and diethylamine (2920mg, 40mmol) were added thereto, and the mixture was heated to reflux for 3h . After the reaction, the reaction solution was poured into ice water, extracted twice with an equal amount of dichloromethane, and the organic phases were combined. The combined organic phases were successively washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to remove the solvent to obtain a crude product. The crude product was purified by silica gel column chromatography (mobile phase: petroleum ether / acetone=100:1.5, v / v), and the concentrated brown elution band was collected and concentrated to give Compound III as a pale yellow solid (246.1mg, 64%) .
[0...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More