Pregna-1,4-diene-3,20-dione, 11,21-bis(acetyloxy)-16,17-dihydroxy-, (11β, 16α)-

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018 - 2019

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2019

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2016

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:

Pregna-1,4-diene-3,20-dione, 11,21-bis(acetyloxy)-16,17-dihydroxy-, (11β, 16α)-

EC Number:

611-417-8

Cas Number:

56723-09-2

Molecular formula:

C25H32O8

IUPAC Name:

Pregna-1,4-diene-3,20-dione, 11,21-bis(acetyloxy)-16,17-dihydroxy-, (11β, 16α)-

Test material form:

solid: particulate/powder

Details on test material:

- Appearance: White powder
- Storage condition of test material: At room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

>= 230.8 - <= 235.1 °C

Decomposition:

yes

Decomp. temp.:

ca. 230 °C

Any other information on results incl. tables

Three experiments were performed to investigate the melting and boiling behaviour of the substance.

DSC EXPERIMENT 1

An endothermic peak was observed between 200°C and 250°C followed by another endothermic effect starting at 250°C (see the illustration below). The extrapolated onset temperature of the first peak was 235.137°C. The first endothermic effect was most likely caused by melting of the test item. The second endothermic effect was probably caused by reaction and/or decomposition of the test item.

After the experiment, a dark 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 2

In order to investigate the melting peak, in Experiment 2 heating was stopped directly after the melting effect. The extrapolated onset temperature was 230.844°C. After the experiment, a light yellow molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test item.

 

DCS EXPERIMENT 3

The difference in the extrapolated onset temperature between Experiment 1 and 2 was >1°C. Therefore a third experiment was performed, applying the same heating rate as in experiments 1 and 2, and the same end temperature as in experiment 2.

The extrapolated onset temperature was 234.398°C. After the experiment, a light yellow molten residue remained in the container.

Experiment 3 thus confirmed melting of the test item, in combination with reaction and/or decomposition.

DATA HANDLING

The melting temperature is reported as a range because of the rather large variantion in values obtained in the three experiments. The variation is likely due to reaction and/or decomposition of the test item.

Applicant's summary and conclusion

Conclusions:

The melting temperature of the substance was determined to be in the range of 230.8°C - 235.1°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 in the range of 230.8°C - 235.1°C.

In the DCS experiments, reaction and/or decomposition of the substance was observed during and after melting, starting at approximately 230°C.