[1R-(1α,2β,5α)]-2-isopropyl-5-methylcyclohexyl 5-oxo-L-prolinate

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:

18 October 2017 - 15 December 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Justification for type of information:

The study was conducted according to an internationally recognised method, and under GLP. The substance is considered to be adequately characterised. Therefore full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Principles of method if other than guideline:

Not applicable

GLP compliance:

yes (incl. QA statement)

Remarks:

GLP certificate (inspected on 15 to 16 November 2017 / signed on 15 May 2018)

Type of method:

capillary method

Remarks:

and DSC method

Melting / freezing pt.:

>= 3.2 - <= 11.7 °C

Atm. press.:

ca. 1 013 hPa

Remarks on result:

other:

Remarks:

Atmospheric pressure not specified, but assumed to be ambient.

Results of the pre-test :

At room temperature, the test item was a not flowable colourless to slightly yellow mass, very viscous and sticky with a ropy consistence.

At 4.2°C, the test item was more solid than at room temperature and at -22.3°C and -80°C the substance was solid like ice.

 

Results of the Main test using DSC method:

In all runs the mass of the crucibles were the same after the measurements and the crucibles were visually unchanged.

 

In the first measurement, no events were observed.

During the cooling down phase,a decreasing of the baseline was observed in the second, third and fourth measurements.

In addition, a small endothermic event was detected in the second measurement but no event was detected in the third and fourth measurements.

During the heating up phase, a small endothermic event was observed between approximately -20°C and 20°C (end of temperature program) in the second, third and fourth measurements.

 

Results of the Main test using Capillary method:

At -10.1 °C a first gluing was noted.

Start of melting was detected using a short piece of thin wire, when the test item started to stick, at 3.2°C (first determination) and 3.1°C (second determination).

End of melting was stated when the short piece of thin wire has totally gone through the test item at 11.8°C (first determination) and 11.5°C (second determination).

Considering that the difference between duplicate determinations was <=0.5 K, the results were considered as valid.

Considering that the difference between begin and end of melting process is > 0.5K, a melting range was stated.

Conclusions:

The melting range of test substance was determined to be between 3.2 and 11.7°C.

Executive summary:

The melting range of the test substance was determined under GLP according to EU Method A.1 and OECD 102 guideline.

A pre-test was conducted, showing that the substance was a not flowable colourless to slightly yellow mass, very viscous and sticky with a ropy consistence at ambient temperature and pressure. Four determinations were carried out using the DSC method, showing that no events can be clearly assigned to a freezing/melting point /range under the experimental conditions used. Finally, the main test was conducted using the Capillary method. Using this method, the melting range, detected with a short piece of thin wire, was determined from 3.2°C to 11.7 °C (276.4 K to 284.9 K) (mean values of two independent determinations).

Description of key information

The melting range of test substance was determined to be between 3.2 and 11.7°C.

The test item was flowable at 60°C.

Additional information

A fully reliable GLP experimental study, conducted according to a recognized OECD/EC guidelines is available.

It is considered as a key study.