2,4-dihydro-4-[4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl]-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:

07 September 2016 - 22 December 2016

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:

2,4-dihydro-4-[4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl]-3H-1,2,4-triazol-3-one

EC Number:

278-009-6

EC Name:

2,4-dihydro-4-[4-[4-(4-methoxyphenyl)piperazin-1-yl]phenyl]-3H-1,2,4-triazol-3-one

Cas Number:

74853-07-9

Molecular formula:

C19H21N5O2

IUPAC Name:

4-{4-[4-(4-METHOXYPHENYL)PIPERAZIN-1-YL]PHENYL}-2,4-DIHYDRO-3H-1,2,4-TRIAZOL-3-ONE

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-1802905-AAA (T001328)
- Physical state: solid
- Appearance: Purple powder

Specific details on test material used for the study:

- Batch n°: I16AB0441
- Expiration date: 30 January 2018
- Analytical purity: 98% and 100% (based on acid and base titration assay respectively)
- Storage condition of test material: At room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

289.9 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

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

Decomp. temp.:

>= 289 °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 380°C. At 407°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: purple). 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 250°C and 300°C. The extrapolated onset temperature of the peak was 289.986°C. The effect was most likely obtained due to melting. The start of an exothermic effect was observed from 325°C. The effect was due to reaction and/or decomposition of the test item. After the experiment, a brown molten residue remained. To investigate the melting peak between 250°C and 300°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 289.905°C. The melting temperature of T001328 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 289.9°C (563.1K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-1802905-AAA (T001328) was determined at 289.9°C (563.1K) by using DSC.