2-[(3S)-2,6-dioxooxan-3-yl]isoindole-1,3-dione

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 03 June 2016 to 11 November 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

2-[(3S)-2,6-dioxooxan-3-yl]isoindole-1,3-dione

EC Number:

607-813-5

Cas Number:

25830-77-7

Molecular formula:

C13 H9 N O5

IUPAC Name:

2-[(3S)-2,6-dioxooxan-3-yl]isoindole-1,3-dione

Test material form:

solid

Details on test material:

- Appearance: white solid
- Storage conditions: in refrigerator (2-8°C) protected from light

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

204 °C

Decomposition:

yes

Decomp. temp.:

204 °C

Remarks on result:

other: Decomposition started during melting.

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

From 250°C upwards the weight of the sample decreased significantly. At 352°C the sample weight had decreased by 25%. After the experiment, a brown/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.

 

DSC EXPERIMENT 1

An endothermic peak between 125°C and 150°C was observed (unknown effect). An endothermic peak between 175°C and 225°C was observed (extrapolated onset temperature: 204.21°C). The effect was most likely obtained due to melting of the test item. An exothermic peak started from 325°C due to reaction and/or decomposition of the test item. After the experiment, a brown/black molten residue remained in the sample container.

 

DSC EXPERIMENT 2

To investigate the melting peak between 175°C and 225°C a repeated heating cycle was applied. With the first heating the extrapolated onset temperature of the melting peak was 204.13°C. During cooling a glass transition was observed between 25°C and 50°C. With the second heating a glass transition was observed between 50°C and 75°C (inflection point: 58.83°C). An exothermic peak between 100°C and 150°C was observed due to crystallization. An endothermic peak between 175°C and 225°C was observed (extrapolated onset temperature: 196.41°C). The effect was most likely obtained due to melting and reaction and/or decomposition of the test item. After the experiment, a yellow molten residue remained in the sample container.

 

DSC EXPERIMENT 3

To investigate the endothermic peak between 125°C and 150°C a repeated heating cycle was applied in the Experiment 3. During cooling no effects were observed. With the second heating no effects were observed. Since no weight loss was observed during the preliminary test between 125°C and 150°C, it is possible but not likely that the endothermic peak was due to evaporation of volatile components. A rearrangement of the crystal structure also might be the reason for this peak. After the experiment, the sample appeared to have been unchanged, i.e. no decomposition and/or evaporation were observed.

 

DSC EXPERIMENT 4

To investigate reaction and/or decomposition during melting, heating was stopped directly after the melting peak. The extrapolated onset temperature of the melting peak was 204.12°C. After the experiment, an off-white molten residue remained in the sample container. This is an indication that reaction and/or decomposition occurred during melting of the test item. 

KEY RESULT

The melting temperature was determined as the average melting temperature obtained from Experiment 1 (204.21°C), Experiment 2 (204.13°C) and Experiment 4 (204.12°C).

Applicant's summary and conclusion

Conclusions:

The melting temperature was determined to be 204°C.

Executive summary:

Differential Scanning Calorimetry (DSC) experiments were performed in a GLP study according to EC A.1, OECD 102 and OPPTS 830.7200. The melting temperature of the substance was determined to be 204°C. Reaction and/or decomposition was observed during and after melting.