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4-[[4-[[4-[(E)-2-cyanoethenyl]-2,6-dimethylphenyl]amino]-2 pyrimidinyl]amino] benzonitrile monohydrochloride

IP.com Disclosure Number: IPCOM000211161D
Publication Date: 2011-Sep-26
Document File: 2 page(s) / 26K

Publishing Venue

The IP.com Prior Art Database

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4-[[4-[[4-[(E)-2-cyanoethenyl]-2,6-dimethylphenyl]amino]-2 pyrimidinyl]amino] benzonitrile monohydrochloride

Chromatographic purity of Edurant tablet

An Edurant tablet was dissolved by sonication in 25 ml of diluent, the resulting solution was filtered through a PTFE filter and injected into the HPLC system.

The HPLC conditions were:

Column & Packing: Ascentis Express C18, Supelco, 2.7 m, 100*3.0

Buffer 0.01 M Ammonium formate adjusted to pH 4.0 with formic acid

Eluent A; 95 : 5, Buffer : Acetonitrile

Eluent B: Acetonitrile
Time % Eluent A % Eluent B 0 95 5
1 95 5
21 55 45
32 40 60

             35 40 60 Equilibrium time: 5 min

Sample volume: 5 L

Flow rate: 0.75 mL/min

Detector: 280 nm

Column
temperature:

Diluent: Methanol

Gradient

55 C


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The obtained results are presented in the table below:

Impurity profile, RRT, % on area

RRT 0.55 RRT 0.59 IMP1 Total

Edurant 99.5 0.21 0.07 0.12 0.4

IMP1 has the following structure:

H

N N

N

H

N

Sample

Purity of 4-[[4-[[4-[(E)-2-

cyanoethenyl]-2,6-

dimethylphenyl]amino]-2

pyrimidinyl]amino]benzonitrile

monohydrochloride

CN

C

N