(+-)-2,4-dihydro-4-[4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl]-2-(1-methylpropyl)-3H-1,2,4-triazol-3-one

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-01-31 to 2017-05-12

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

1-(butan-2-yl)-4-{4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl}-4,5-dihydro-1H-1,2,4-triazol-5-one

EC Number:

607-685-0

Cas Number:

252964-68-4

Molecular formula:

C23H29N5O2

IUPAC Name:

1-(butan-2-yl)-4-{4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl}-4,5-dihydro-1H-1,2,4-triazol-5-one

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study report): JNJ-7982559-AAA (T001329)
- Physical state: solid (powder)
- Appearance: Grey-brown powder

Specific details on test material used for the study:

- Batch n°: I14IB3639
- Analytical purity: 97.9% (based on HPLC)
- Expiration date: 2020-09-17
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

197.8 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.

Decomp. temp.:

> 375 °C

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 400°C. At 422°C the sample weight has decreased by 25%. After the experiment, a dark brown molten residue remained in the sample container (original colour: grey brown). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 175°C and 225°C. The extrapolated onset temperature of the peak was 197.7°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 375°C due to reaction and/or decomposition of the test item. After the experiment, a brown molten residue remained. To investigate the melting peak between 175°C and 225°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 197.9°C. The melting temperature of T001329 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 197.8°C (471.0K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-7982559-AAA (T001329) was determined at 197.8°C (471.0K) by using DSC.