L-Leucine, 4-fluoro-N-[(1S)-2,2,2-trifluoro-1-[4'-(methylsulfonyl)[1,1'-biphenyl]-4-yl]ethyl]-, compd. with N-cyclohexylcyclohexanamine (1:1)

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

December 16, 2011 - January 27, 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: This study has been performed according to OECD 102 (1995), EU Method A.1 (2008), EPA OPPTS 830.7200 (1998) and according to GLP principles.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

(1995)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

(2008)

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 (incl. QA statement)

Type of method:

thermal analysis

Remarks:

(differential scanning calorimetry (DSC))

Test material

Test material information

Constituent 1

Reference substance name:

N-cyclohexylcyclohexanaminium (2S)-4-fluoro-4-methyl-2-{[(1S)-2,2,2-trifluoro-1-{4'-methanesulfonyl-[1,1'-biphenyl]-4-yl}ethyl]amino}pentanoate

EC Number:

700-778-8

Cas Number:

1064076-86-3

Molecular formula:

C21H23F4NO4S.C12H23N

IUPAC Name:

N-cyclohexylcyclohexanaminium (2S)-4-fluoro-4-methyl-2-{[(1S)-2,2,2-trifluoro-1-{4'-methanesulfonyl-[1,1'-biphenyl]-4-yl}ethyl]amino}pentanoate

Details on test material:

- Name of test material (as cited in study report): Biphenyl DCHA Salt
- Description: White powder

Results and discussion

Melting / freezing point

Melting / freezing pt.:

208 °C

Any other information on results incl. tables

Preliminary test

From 200°C upwards the weight of the sample decreased significantly. At 311°C the sample weight had decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test substance.

Main study (1st experiment)

An endothermic peak directly followed by an exothermic effect was observed between 175°C and 250°C. The extrapolated onset temperature of the endothermic peak was 207.63°C. The effects were most likely obtained due to melting followed by reaction and/or decomposition of the test substance. After the experiment, an orange molten residue remained in the sample container.

Main study (2nd experiment)

To investigate melting of the test substance the second experiment was stopped at 215°C i.e. during the endothermic effect. After the experiment, a colourless molten residue remained in the sample container. This is an indication that the endothermic effect was due to melting of the test substance.

Main study (3rd experiment)

The third experiment was performed to determine as a duplicate of the first experiment.Similar results as with the first experiment were obtained. The extrapolated onset of the melting peak was 207.42°C. After the experiment, a yellowish molten residue remained in the sample container. This is an indication that reaction and/or decomposition occurred directly after melting.

Applicant's summary and conclusion

Conclusions:

The melting temperature of the substance (a solid under ambient conditions) was determined using DSC in accordance with OECD 102 (1995), EU Method A.1 (2008), EPA OPPTS 830.7200 (1998) and according to GLP principles. The melting temperature of the test substance was 208°C (481K).