2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-ylmethyl)-1,3-dioxolane-4-methanol

Melting point / freezing point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

supporting study

Reliability:

4 (not assignable)

Rationale for reliability incl. deficiencies:

other: Documentation insufficient for assessment. No information on purity of the substance.

GLP compliance:

not specified

Type of method:

thermal analysis

Melting / freezing pt.:

142 °C

Conclusions:

The melting point of the T001159 is 142 deg C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

03 September - 15 December 2015

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°: M14IB5308
- Analytical purity: 99.6%
- Expiration date: 03 February 2016
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

140.6 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A black molten residue remained after the preliminary and the first experiment of the main test and a beige molten residue after the second experiment, indicating reaction and/or decomposition.

Decomp. temp.:

> 300 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly from 350°C. At 370°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: off-white). 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 125°C and 175°C. The extrapolated onset temperature of the peak was 140.60°C. The effect was most likely obtained due to melting. An exothermic peak was observed starting at 300°C due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained. To investigate the melting peak between 125°C and 175°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 140.61°C. After the experiment, a beige molten residue remained in the sample container. Since no colour change was observed, it could be concluded that the endothermic effect was due to melting of the test item.

The melting temperature of T001159 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 140.6°C (413.8K).

Conclusions:

The melting temperature of JNJ-16479489-AAA (T001159) was determined to be 140.6°C (413.8K) by using DSC.

Description of key information

In a GLP study according to OECD guideline 102, EU method A.1 and EPA OPPTS 830.7200 (K1, Reingruber, 2016) the melting point of T001159 was determined to be 140.6°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

140.6 °C

Additional information

A supporting study (Pharmaceutical Science) with insufficient documentation, and therefore assigned as K4, concluded that the melting temperature of T001159 is 142.0°C which is in line with the result of the key study.