Benzonitrile, 4-[(4-chloro-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:

28 December 2015 - 25 April 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 (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

- Batch n°: I15FC2164
- Analytical purity: 102.2% (HPLC assay)
- Expiration date: 23 June 2017
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

216.1 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A charred molten residue remained after the preliminary and the first main test and a yellowish molten test item was observed after the second main test, indicating reaction and/or decomposition

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 225°C. At 466°C the sample weight has decreased by 25%. After the experiment, a charred molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

Main test

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 200°C and 230°C. The extrapolated onset temperature of the peak was 216.15°C. The effect was most likely obtained due to melting. This effect was followed by an exothermic effect between 230°C and 250°C. The latter was most likely obtained due to reaction and/or decomposition of the test item. Another exothermic effect was seen between 300°C and 350°C. This effect was most likely due to further reaction and/or decomposition of the test item. After the experiment, a charred molten residue remained.

To investigate the melting peak between 200°C and 230°C, a repeated heating cycle was applied with a lower end temperature (i.e. 230°C). The extrapolated onset temperature of the melting peak was 216.07°C. After the experiment it was observed that the test item was molten and yellowish. The change of colour and state of matter indicated melting in combination with reaction and/or decomposition.

The melting temperature of T002488 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 216.1°C (489.3K).

Conclusions:

The melting temperature of JNJ-4754724-AAA (T002488) was determined to be 216.1°C (489.3K) using DSC.

Reaction and/or decomposition of JNJ-4754724-AAA (T002488) was observed simultaneously with melting during the DSC experiments.

Description of key information

In a GLP study according to OECD guideline 102, EU method A.1 and EPA OPPTS 830.7200 (Klimisch 1, Reingruber, 2016) the melting point of T002488 was determined to be 216.1°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

216.1 °C