Glycyrrhetinic acid cyclic phosphonate ester derivative and preparation method thereof
A technology of glycyrrhetinic acid and its products, which is applied in the field of glycyrrhetinic acid cyclic phosphate derivatives and its preparation, can solve problems such as difficulty in maintaining stable blood drug concentration and tissue drug concentration, affecting drug efficacy, and short half-life, achieving significant relief. release performance, improve drug efficacy, and facilitate synthesis
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0013] Cis-3-O-[4-(R)-(3-chlorophenyl)-2-oxo-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid methyl of the present invention Esters (i.e. R 1 is methyl, R 2 It is 3-chlorophenyl, and the 4-position of the phosphorus heterocyclic ring is a glycyrrhetinic acid cyclic phosphate derivative of R type) and cis-3-O-[4-(S)-(3-chlorophenyl)-2-oxo Generation-1,3,2-dioxaphosphorinyl]-18β-methyl glycyrrhetinate (ie R 1 is methyl, R 2 It is 3-chlorophenyl, and the 4-position of phosphorus heterocycle is the preparation of the glycyrrhetinic acid cyclic phosphate derivative of S type):
[0014] cis-3-O-[4-(R)-(3-chlorophenyl)-2-oxo-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid methyl ester
[0015] Weigh 0.44g (0.906mmol) of methyl glycyrrhetinate, put it in a 25mL eggplant-shaped bottle, add 5mL of anhydrous tetrahydrofuran to dissolve, add 2mol / L of N,N-diisopropylamide lithium in tetrahydrofuran solution 2.3mL (4.6mmol), stirred at room temperature for 1h. Weigh the known trans...
Embodiment 2
[0024] Cis-3-O-[4-(R)-(3-chlorophenyl)-2-oxo-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid ( i.e. R 1 for hydrogen, R 2 It is 3-chlorophenyl, and the 4-position of the phosphorus heterocyclic ring is a glycyrrhetinic acid cyclic phosphate derivative of R type) and cis-3-O-[4-(S)-(3-chlorophenyl)-2-oxo Generation-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid (i.e. R 1 for hydrogen, R 2 It is 3-chlorophenyl, and the 4-position of phosphorus heterocycle is the preparation of the glycyrrhetinic acid cyclic phosphate derivative of S type):
[0025] cis-3-O-[4-(R)-(3-chlorophenyl)-2-oxo-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid
[0026] Weigh 1.26g (2.68mmol) of glycyrrhetinic acid, put it in a 100mL eggplant-shaped bottle, add 30mL of anhydrous tetrahydrofuran to dissolve, add 2mol / L of N, N-diisopropylamide lithium tetrahydrofuran solution 6.7mL (13.4 mmol), stirred at room temperature for 2h. Weigh the known trans-4-(R)-(3-chlorophenyl)-2-(4-nitrophenoxy)-2-oxo...
Embodiment 3
[0039] The preparation of the glycyrrhetinic acid substituted by different substituents of the present invention:
[0040] cis-3-O-[4-(R)-phenyl-2-oxo-1,3,2-dioxaphosphorinyl]-18β-glycyrrhetinic acid
[0041] Starting from the known trans-4-(R)-phenyl-2-(4-nitrophenoxy)-2-oxo-1,3,2-dioxaphosphorinane, instead of Trans-4-(R)-(3-chlorophenyl)-2-(4-nitrophenoxy)-2-oxo-1,3,2-dioxaphosphorane in Example 2 Hexane was reacted, and other reaction reagents and experimental operations were the same as in Example 2 to obtain 0.82 g of a light yellow powder product, with a yield of 43.0%, a melting point greater than 200 ° C, and a specific rotation of +93.0 ° (c 1.000, CHCl 3 ). MS (ES + ): m / z=667.6[M+H + ].
[0042] The proton nuclear magnetic resonance spectrum, carbon spectrum and phosphorus spectrum data of the compound obtained are respectively: 1 H NMR (600MHz, CDCl 3 , only list the chemical shift value of characteristic hydrogen) δ: 7.41-7.34 (m, 5H), 5.71 (s, 1H), 5.41 (...
PUM
| Property | Measurement | Unit |
|---|---|---|
| optical rotation | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
| specific rotation | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More 