1-[3-(Hydroxymethyl)pyridin-2-yl)-4-methyl-2-phenylpiperazine

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 January 2018 - 02 August 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

{2-[(2R)-4-methyl-2-phenylpiperazin-1-yl]pyridin-3-yl}methanol; {2-[(2S)-4-methyl-2-phenylpiperazin-1-yl]pyridin-3-yl}methanol

EC Number:

700-296-8

Cas Number:

61337-89-1

Molecular formula:

C17-H21-N3-O

IUPAC Name:

{2-[(2R)-4-methyl-2-phenylpiperazin-1-yl]pyridin-3-yl}methanol; {2-[(2S)-4-methyl-2-phenylpiperazin-1-yl]pyridin-3-yl}methanol

Test material form:

solid: particulate/powder

Details on test material:

Physical appearance: white powder
Storage conditions: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

121.4 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

275 °C

Remarks on result:

other: Decomposition started after melting.

Any other information on results incl. tables

Two experiments were performed to investigate the melting (and boiling) behaviour of the substance.

 

DSC EXPERIMENT 1

An endothermic peak was observed between 100°C and 150°C followed by another endothermic effect starting at ca. 275°C. The extrapolated onset temperature of the peak was 121.715°C. This endothermic effect was most likely caused by melting of the test item. The second endothermic effect was probably due to reaction and/or decomposition of the test item.

After the experiment, a yellow molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was concluded that the test item had molten and that the change of the colour demonstrated reaction and/or decomposition of the test item.

 

DSC EXPERIMENT 2

In order to investigate the melting peak, in Experiment 2 heating was stopped directly after the melting peak. The extrapolated onset temperature was 121.102°C. 

After the experiment, a white molten residue remained in the sample container. It demonstrated that melting was the reason for the endothermic effect.

 

DATA HANDLING

The melting temperature was determined as the mean melting temperature of Experiment 1 (121.715°C) and Experiment 2 (121.102°C).

 

TGA and DSC curve recorded during heating: see Illustration

Applicant's summary and conclusion

Conclusions:

The melting temperature of the substance was determined to be 121.4°C.

Executive summary:

Differential Scanning Calorimetry (DSC) experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200.

The melting temperature of the substance was determined in duplicate obtaining a mean value of 121.4°C.

Reaction and/or decomposition of the substance was observed at temperatures > 275°C.