cis-2-(2,4-dichlorophenyl)-2-(1H-imidazol-1-ylmethyl)-1,3-dioxolane-4-ylmethyl methanesulphonate monohydrochloride

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:

24 August 2015 - 25 August 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°: I14KB4717
- Analytical purity: 105.7% (acid titration)
- Expiration date: 25 November 2016
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

166.6 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 250 °C

Remarks on result:

other: A black expanded residue was observed after the experiment, indicating reaction and/or decomposition of the test item

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 300°C. At 357°C the sample weight had decreased by 25%. After the experiment, a black expanded residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In the first experiment a DSC curve with an endothermic peak between 125°C and 200°C was obtained. The extrapolated onset temperature of the peak was 166.58°C. The effect was most likely obtained due to melting. A exothermic signal was observed starting at 250°C due to reaction and/or decomposition of the test item. After the experiment, a black expanded residue remained.

To investigate the melting peak between 125°C and 200°C, a repeated heating cycle was applied up to 200°C and thus stopped directly after the endothermic peak. The extrapolated onset temperature of the melting peak was 166.74°C. In the third experiment, the extrapolated onset temperature of the peak was 166.60°C. After the experiment, a colourless molten residue remained in the sample container. The result demonstrated that the endothermic effect was due to melting of the test item. The melting temperature of T001202 as the average melting temperature from Experiment 1 (166.58°C), Experiment 2 (166.74°C) and Experiment 3 (166.60°C) was determined to be 166.6°C (440K) by using DSC. Reaction and/or decompostion of T001202 was observed starting at > 250°C (> 523K).

Conclusions:

The melting temperature of JNJ-17336007-AAC (T001202) was determined at 166.6°C (440K) by using DSC.
Reaction and/or decomposition was observed at temperatures of > 250°C (> 523K).

Description of key information

In a GLP study according to OECD guideline 102, EU method A.1 and EPA OPPTS 830.7200 (Klimisch 1, Ciric, 2017) the melting point of T001202 was determined at 166.6°C (440K) by using DSC.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

166.6 °C