3,20-bis(ethylenedioxy)pregna-5,7-diene

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

18/12/2012 - 12/3/2013

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted following OECD/EU guideline and in accordance with GLP. Study material is well characterized.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2013

Report date:

2013

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Remarks:

DSC

Test material

Test material information

Constituent 1

Reference substance name:

3,20-bis(ethylenedioxy)pregna-5,7-diene

EC Number:

243-175-0

EC Name:

3,20-bis(ethylenedioxy)pregna-5,7-diene

Cas Number:

19592-55-3

Molecular formula:

C25H36O4

IUPAC Name:

(1S,3aR,9aR,9bS,11aS)-9a,11a-dimethyl-1-(2-methyl-1,3-dioxolan-2-yl)-1,2,3,3a,6,8,9,9a,9b,10,11,11a-dodecahydrospiro[cyclopenta[a]phenanthrene-7,2'-[1,3]dioxolane]

Test material form:

solid: crystalline

Details on test material:

- Name of test material (as cited in study report): Proketal; pregna-5,7-diene-3,20-dione, cyclic 3,20-bis(1,2-ethanediyl acetal)
- Substance type: Intermediate
- Physical state: Powder
-

Results and discussion

Melting / freezing point

Melting / freezing pt.:

ca. 187 °C

Atm. press.:

ca. 1 Bar

Decomposition:

ambiguous

Decomp. temp.:

> 250 °C

Any other information on results incl. tables

The extrapolated onset temperature of the peak was 187.26°C. The effect was most likely obtained due to melting of the test substance. A small endothermic effect between 200°C and 225°C was observed, this effect was obtained due to unknown reasons. This effect was followed by a broad endothermic effect starting at 250°C. The latter was most likely obtained due to reaction and/or decomposition of the test substance. After the experiment, a brown molten residue remained in the sample container.

To investigate the melting peak between 150°C and 225°C a repeated heating cycle was applied in experiment 2. With the first heating the extrapolated onset temperature of the melting peak was 187.21°C. The similar value indicated that melting of the test substance was the reason for the effect.

During cooling an exothermic peak was observed between 120°C and 100°C. The effect was obtained due to crystallization of the test substance.

With the second heating an extrapolated onset temperature of 173.78°C was obtained. The results demonstrated that the endothermic effect was due to melting of the test substance. After the experiment, a brown molten residue remained in the sample container.

Applicant's summary and conclusion

Conclusions:

The melting and boiling temperature of Proketal were determined using DSC. The melting temperature of the test substance was 187°C (460K).