Reaction mass of 2,6-Bis[(dimethylamino)methyl]-4-(1-{3-[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)phenol and 4-(1-{3,5-Bis[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)-2,6-bis[(dimethylamino)methyl]phenol

Stability in organic solvents and identity of relevant degradation products

Administrative data

Endpoint:

stability in organic solvents and identity of relevant degradation products

Remarks:

solvent: ethanol

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

study well documented, meets generally accepted scientific principles, acceptable for assessment

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2015

Report date:

2015

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: SOP 00191, Version 2

Version / remarks:

SOP (Standard Oparating Procedure) by CURRENTA GmbH, Leverkusen, Germany

Principles of method if other than guideline:

Homogeneity: Visual inspection
Stability: Calculation of the recovery of the test item in ethanol based on the peak Mannich Base (4x, 3x, 2x substituted). The quantification was performed by HPLC-MS

GLP compliance:

yes

Test material

Test material information

Constituent 1

Reference substance name:

4-(1-{3,5-Bis[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)-2,6-bis[(dimethylamino)methyl]phenol

Molecular formula:

C27H44N4O2

IUPAC Name:

4-(1-{3,5-Bis[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)-2,6-bis[(dimethylamino)methyl]phenol

Constituent 2

Reference substance name:

2,6-Bis[(dimethylamino)methyl]-4-(1-{3-[(dimethylamino)methyl]-4-hydroxyphenyl}- 1-methylethyl)phenol

Molecular formula:

C24H37N3O2

IUPAC Name:

2,6-Bis[(dimethylamino)methyl]-4-(1-{3-[(dimethylamino)methyl]-4-hydroxyphenyl}- 1-methylethyl)phenol

Constituent 3

Reference substance name:

2-[(Dimethylamino)methyl]-4-(1-{3-[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)phenol

Molecular formula:

C21H30N2O2

IUPAC Name:

2-[(Dimethylamino)methyl]-4-(1-{3-[(dimethylamino)methyl]-4-hydroxyphenyl}-1-methylethyl)phenol

impurity 1

Reference substance name:

Unknown impurities

IUPAC Name:

Unknown impurities

impurity 2

Reference substance name:

Xylene

EC Number:

215-535-7

EC Name:

Xylene

Cas Number:

1330-20-7

Molecular formula:

C8H10

IUPAC Name:

Benzene, dimethyl-

impurity 3

Reference substance name:

Water

EC Number:

231-791-2

EC Name:

Water

Cas Number:

7732-18-5

Molecular formula:

H2O

IUPAC Name:

water

impurity 4

Reference substance name:

Sulphated ash

IUPAC Name:

Sulphated ash

Test material form:

solid: bulk

Details on test material:

- Name of test material (as cited in study report): HPP 12879-1

Results and discussion

Test substance stable:

yes

Remarks:

According to SOP 00191 Version 2, the 0.01 mg/mL and 423 mg/mL formulation of the test item in ethanol are homogeneous and stable for at least 24 hour at room temperature.

Any other information on results incl. tables

Homogeneity:

The formulation 0.01 mg/mL and 423 mg/mL are clear solutions and therefore homogeneous.

Stability:

Calculation of recovery of the test item in ethanol based on peak Mannich Base (4x substituted)

Nominal value mg/mL	Theoretical value Mg/mL	Content test item mg/mL		Recovery as % of theoretical value
		Start	After 24 hours	Start	After 24 hours
0.01	0.0101	0.0102	0.0098	101	97
423	423	419	430	99	101

 

Calculation of recovery of the test item in ethanol based on peak Mannich Base (3x substituted)

Nominal value mg/mL	Theoretical value Mg/mL	Content test item mg/mL		Recovery as % of theoretical value
		Start	After 24 hours	Start	After 24 hours
0.01	0.0101	0.0103	0.0104	102	103
423	423	432	424	102	100

 

Calculation of recovery of the test item in ethanol based on peak Mannich Base (2x substituted)

Nominal value mg/mL	Theoretical value Mg/mL	Content test item mg/mL		Recovery as % of theoretical value
		Start	After 24 hours	Start	After 24 hours
0.01	0.0101	0.0104	0.0101	103	100
423	423	435	445	103	105

 

Applicant's summary and conclusion

Conclusions:

The 0.01 mg/mL and 423 mg/mL formulations of HPP 12879-1 in ethanol are homogeneous and stable for at least 24 hours at room temperature.

Executive summary:

According to SOP 00191 Version 2, the 0.01 mg/mL and 423 mg/mL formulations of HPP 12879 -1 in ethanol are clear and therefore homogeneous. They are stable for at least 24 hour at room temperature.