Benzonitrile, 4-[(1,6-dihydro-4-hydroxy-6-oxo-2-pyrimidinyl)amino]-

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:

14 July 2015 - 23 February 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°: I15BB0824
- Analytical purity: 99.6%
- Expiration date: 28 August 2015
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

265.7 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

Reaction and/or decomposition was observed during melting of the test item. After the experiments, a purple molten residue remained in the sample container, indicating reaction and/or decomposition.

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 275°C. At 465°C the sample weight has decreased by 25%. After the experiment, a charred and expanded residue remained in the sample container (original colour: slight beige). 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 showed an endothermic peak between 100°C and 150°C. The effect was most likely obtained due to evaporation of volatile components (i.e. solvent, impurities). An endothermic effect with two peaks followed by an exothermic effect was observed between 250°C and 350°C. The extrapolated onset temperature of the first endothermic peak was 265.84°C. The effects were most likely obtained due to melting and reaction and/or decomposition of the test item. After the experiment, a purple molten residue remained in the sample container.

To investigate the melting peak, experiment 2 was stopped directly after the first endothermic peak at 285°C. The extrapolated onset temperature of the melting peak was 265.52°C. After the experiment, an orange molten residue remained in the sample container. It demonstrated that melting and reaction and/or decomposition of the test item was the reason for the endothermic effect.

Experiment 3 was performed to observe if decomposition occurs before melting. Since no changes were observed after the experiment it can be concluded that the endothermic peak between 100°C and 175°C is due to evaporation of volatile components (i.e. solvent, impurities) and that no decomposition occurred before melting of the test item.

The melting temperature was determined as the average melting temperature obtained from experiment 1 (265.84°C) and experiment 2 (265.52°C).

Conclusions:

The melting temperature of JNJ-4370561-AAA (T002326) was determined at 265.7°C (539K) by using DSC.
Reaction and/or decomposition of the substance was observed during melting of the test item.

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 (K1, Reingruber, 2016). The melting point of T002326 was determined to be 265.7°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

265.7 °C

Additional information

Reaction and/or decomposition was observed during melting.