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Physical & Chemical properties

Melting point / freezing point

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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

Additional information