.alpha.-D-Glucopyranosyl bromide, 2,3,4,6-tetrakis(2,2-dimethylpropanoate)

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:

19 December 2016 - 07 July 2017

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°: M16FB2273
- Analytical purity: 101.7% (w/w)
- Expiration date: 12 September 2017
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

147.5 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 225 °C

Remarks on result:

other: A brown molten residue remained after the preliminary and first main test, indicating reaction and/or decomposition. A white molten residue remained after the second main test indicating melting.

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 225°C. At 263°C the sample weight has decreased by 25%. After the experiment, a brown 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 was obtained and showed an endothermic peak between 125°C and 175°C. The extrapolated onset temperature of the peak was 147.749°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 225°C due to reaction and/or decomposition of the test item. After the experiment, a  brown molten residue remained. To investigate the melting peak between 125°C and 175°C, a repeated heating cycle was applied and directly stopped at 165°C. The extrapolated onset temperature of the melting peak was 147.311°C. The melting temperature of T003421 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 147.5°C (420.7K).

Conclusions:

The melting temperature of JNJ-42808389-AAA (T003421) was determined at 147.5°C (420.7K) 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 J, 2017). The melting point of T003421 was determined to be 147.5°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

147.5 °C