D-Glucitol, 1,5-anhydro-1-C-[3-[[5-(4-fluorophenyl)-2-thienyl]methyl]-4-methylphenyl]-, 2,3,4,6-tetrakis(2,2-dimethylpropanoate), (1S)-

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:

25 May 2016 - 09 Sep 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)

Remarks:

Attached in the study report

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

- Batch n°: I15AB0305
- Analytical purity: 99.7%
- Expiry/retest date: 23/01/2017
- Test item storage conditions: At room temperature

Key result

Melting / freezing pt.:

141.7 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 200 °C

Remarks on result:

other: a black molten residue remained after the preliminary test and a dark brown residue after the main study up to 380°C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly from 325°C. At 380°C the sample weight has decreased by 25%. After the experiment, a black 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 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 125°C and 175°C. The extrapolated onset temperature of the peak was 141.57°C. The effect was most likely obtained due to melting. Small endothermic peaks were observed starting at 200°C due to reaction and/or decomposition of the test item. After the experiment, a dark brown molten residue remained.

To investigate the melting peak, the temperature program of the second experiment was stopped after the endothermic effect. The extrapolated onset temperature of the melting peak was 141.77°C. After the experiment, a white molten residue remained in the sample container.  

The melting temperature for T003422 was determined as the average melting temperature obtained from Experiment 1 (141.57°C) and Experiment 2 (141.77°C) and equals 141.7°C (415K).

Conclusions:

The melting temperature of JNJ-42808415-AAA (T003422) was determined at 141.7°C (415K) by using DSC.

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, Ciric, 2017). The melting point of T003422 was determined to be 141.7°C by using differential scanning calorimetry.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

141.7 °C