tak-875 analogue and its preparation method and application
A TAK-875, 1. The technology of TAK-875 is applied in the field of TAK-875 analogs and its preparation, which can solve the problems of further improvement of drug efficacy and pharmacokinetics
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0060] The synthesis of the key intermediate (S)-2-(6-hydroxy-2,3-chroman-3-yl)methyl acetate (8) and the synthesis reference of the reference drug 1 (TAK-875) have been published literature (WO 2012 / 111849 A1).
[0061] 2-((3S)-6-((2',6'-dimethyl-4'-(3-(methylsulfinyl)propoxy)biphenyl-3-yl)methoxy)- Synthesis of 2,3-chroman-3-yl)acetic acid (11):
[0062] (1) Synthesis of 3-(methylthio)propyl 4-benzenesulfonic acid methyl ester (2):
[0063] Weigh p-toluenesulfonyl chloride (11.2g) into a 250mL reaction flask, add 100mL of anhydrous dichloromethane, then add 12mL of triethylamine, add 3-methylthiopropanol (4.0mL) dropwise at room temperature, and react at 30°C overnight. Add a large amount of dichloromethane, wash with 2M hydrochloric acid until acidic, wash twice with saturated sodium chloride solution, dry over anhydrous magnesium sulfate, pass through a flash column with ethyl acetate / petroleum ether system, and evaporate to dryness to obtain 8.0 g of a colorless oily l...
Embodiment 2
[0077] 2-((S)-6-((2',6'-dimethyl-4'-(3-((S)-methylsulfinyl)propoxy)biphenyl-3-yl)methyl Oxy)-2,3-chroman-3-yl)acetic acid (12) and 2-((S)-6-((2',6'-dimethyl-4'-(3- Preparation of ((R)-methanesulfinyl)propoxy)biphenyl-3-yl)methoxy)-2,3-chroman-3-yl)acetic acid (13).
[0078] The chiral preparation of compound 11 was carried out at Daicel Pharmaceutical Chiral Technology Co., Ltd. Chiral preparation conditions: [column, CHIRALPAK ADH, 0.46cm I.D. × 25cm L; mobile phase, CO 2 / MeOH=60 / 40 (V / V); flow rate, 2.0 mL / min; detection, UV 208 nm; temperature, 35°C]. The retention times were 14.2 minutes and 17.6 minutes, respectively. (S,S)-isomer 12, 100.0% de. [Column, CHIRALPAK IA (4.6mm I.D.×250mm.5um); Mobile phase, n-hexane / ethanol / EtOAc / TFA=75 / 10 / 15 / 0.1 (V / V / V / V); Flow rate, 0.8mL / min; detection, UV 286nm; temperature, room temperature]; [α] 25 D +35.93°(c 0.8, acetonitrile).IR(KBr) 3423,2918,2579,1717,1618,1600,1496,1470,1316,1275,1182,1154,1005,826,797,712,632. 1 H NMR (...
Embodiment 3
[0080] 2-((S)-6-((2',6'-dimethyl-4'-(3-((S)-methylsulfinyl)propoxy)biphenyl-3-yl)methyl Oxy)-2,3-chroman-3-yl)acetic acid (16) or 2-((S)-6-((2',6'-dimethyl-4'-(3- Synthesis of ((R)-methylsulfinyl)propoxy)biphenyl-3-yl)methoxy)-2,3-chroman-3-yl)acetic acid (17):
[0081] (1) Synthesis of 3-(methylthio)propyl 4-benzenesulfonic acid methyl ester, with reference to the steps described in Example 1;
[0082] (2) Synthesis of 4'-hydroxy-2',6'-dimethylbiphenyl-3-carbaldehyde, refer to the steps described in Example 1;
[0083] (3) Synthesis of 2',6'-dimethyl-4'-(3-(methylthio)propoxy)biphenyl-3-carbaldehyde, refer to the steps described in Example 1;
[0084] (4) Synthesis of (2',6'-dimethyl-4'-(3-(methylthio)propoxy)biphenyl-3-yl)methanol, refer to the steps described in Example 1;
[0085] (5)(S)-2-(6-((2',6'-dimethyl-4'-(3-(methylthio)propoxy)biphenyl-3-yl)methoxy )-2,3-benzodihydrofuran-3-yl) methyl acetate synthesis, with reference to the steps described in Example 1;
[00...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


