1-benzhydrylpiperazine

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 January - 04 May 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

- Batch n°: M15BB1451
- Analytical purity: 98.8% (base titration)
- Expiration date: 30 January 2021
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

92.2 °C

Atm. press.:

ca. 1 026 hPa

Decomposition:

yes

Decomp. temp.:

>= 200 - <= 250 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 225°C. At 299°C the sample weight had decreased by 25%. After the experiment, a brown molten residue remained in the sample container (original colour: white to slight beige). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

The DSC curve with a heating rate of 20°C/min showed an endothermic peak between 75°C and 125°C. The extrapolated onset temperature of the peak was 92.11°C. The effect was most likely obtained due to melting. A second endothermic effect was observed between 225°C and 350°C due to decomposition of the test item between 200 and 250°C. After the experiment, a brown molten residue remained.

To investigate the melting peak between 75°C and 125°C, a repeated heating cycle (up to 120°C) in combination with a hermetically sealed sample pan (in order to investigate the boiling point) was applied in the 2nd experiment. The extrapolated onset temperature of the melting peak was 91.90°C. After the experiment, a brown molten residue remained in the sample container.

In the third experiment, the sample was heated up to 120°C. The extrapolated onset temperature of the melting peak was 92.55°C. The visual inspection showed that the test item had melted.

A fourth experiment was performed as a duplicate of experiment 1. Similar results were obtained. The extrapolated onset of the melting peak was 92.29°C, while the second endothermic peak is most likely caused by reaction and/or decomposition starting between 200 and 250°C. After the experiment, a brown molten residue remained in the sample container.

The melting temperature of T000750 as the average melting temperature from Experiment 1 (92.11°C), Experiment 2 (91.90°C), Experiment 3 (92.55°C) and Experiment 4 (92.29°C) was determined to be 92.2°C (365.4K) by using DSC. Reaction and/or decompostion of T000750 was observed between 200 and 250°C (between 473.2 and 523.2K).

Conclusions:

The melting temperature of JNJ-130806-AAA (T000750) was determined to be 92.2°C (365.4K) by using DSC.
Reaction and/or decomposition was observed starting at a temperature between 200 and 250°C (between 473.2 and 523.2K).

Description of key information

A GLP study was performed according to OECD guideline 102, EU Method A.1 and EPA OPPTS 830.7200 without deviations (Brekelmans, 2017). The melting point of T000750 was determined to be 92.2°C 365.4K) by using DSC.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

92.2 °C

Additional information

Reaction and/or decomposition was observed during DSC experiments starting at a temperature between 200 and 250°C (between 473.2 and 523.2K).