1-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2021-02-01 to 2021-07-14

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2021

Report date:

2021

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:

1996

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-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Cas Number:

1903010-39-8

Molecular formula:

C25H23N7O5

IUPAC Name:

1-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Test material form:

solid: particulate/powder

Details on test material:

- Physical state: solid
- Appearance: orange powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Batch (Lot) Number: I20ED2016
- Purity/Composition: 101.5%
- Purity test date : 2020-05-27
- Expiry date: 2022-06-06 (retest date)
- Physical Description: Orange powder

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability and homogeneity of the test material in the vehicle/solvent under test conditions and during storage: not indicated
- Stability in the medium, i.e. sensitivity of the test material to hydrolysis and/or photolysis: not indicated
- Solubility and stability of the test material in the solvent/vehicle and the exposure medium: not indicated
- Reactivity of the test material with the incubation material used (e.g. plastic ware): not indicated

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Final preparation of a solid: not applicable, the solid test item was transferred directly into the DSC cell

OTHER SPECIFICS
- Purity/Composition correction factor: Yes, correction factor is 1.0

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

234.7 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

325 °C

Any other information on results incl. tables

Preliminary Test
Starting at 275°C, the weight of the sample decreased significantly. At 395°C, the sample weight had decreased by 25%.

After the experiment, a black molten and expanded residue remained in the sample container (original colour: orange). The change of the colour indicated reaction and/or decomposition of the test item.

Main Study
In Experiment 1 an endothermic effect directly followed by an exothermic effect was observed between 225°C and 325°C. The extrapolated onset temperature of the endothermic effect was 234.651°C. The endothermic effect was most likely obtained due to melting of the test item. The exothermic effect was due to reaction and/or decomposition of the test item.

After the experiment, a dark brown/black molten residue remained in the sample container (original colour: orange). Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, Experiment 2 was stopped directly after the
melting effect. The extrapolated onset temperature was 234.821°C. After the experiment, an orange/red molten residue remained in the sample container (original colour: orange). It demonstrated that melting and reaction and/or decomposition was the reason for the endothermic effect.

The melting temperature was determined as the mean melting temperature of Experiment 1 (234.651°C) and Experiment 2 (234.821°C).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-73848255-AAA (T003902) was determined by DSC. The melting temperature of the test item was 234.7°C (507.9K). Reaction and/or decomposition of the test item was observed during DSC experiments during and after melting.