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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
05 Dec 2017 - 14 Dec 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report date:
2018

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2016
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
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

Constituent 1
Chemical structure
Reference substance name:
(2R)-5-methoxy-N-propyl-1,2,3,4-tetrahydronaphthalen-2-amine hydrochloride
Cas Number:
93601-85-5
Molecular formula:
C14H21NO.HCl
IUPAC Name:
(2R)-5-methoxy-N-propyl-1,2,3,4-tetrahydronaphthalen-2-amine hydrochloride
Constituent 2
Chemical structure
Reference substance name:
(2S)-5-methoxy-N-propyl-1,2,3,4-tetrahydronaphthalen-2-amine hydrochloride (1:1)
EC Number:
695-797-0
Cas Number:
93601-86-6
Molecular formula:
C14H21NO.HCl
IUPAC Name:
(2S)-5-methoxy-N-propyl-1,2,3,4-tetrahydronaphthalen-2-amine hydrochloride (1:1)
Test material form:
solid: particulate/powder
Details on test material:
- Appearance: White to off-white powder
- Storage condition of test material: At room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
>= 262.6 - <= 265.3 °C
Decomposition:
yes
Remarks on result:
other: Decomposition started during melting.

Any other information on results incl. tables

TGA EXPERIMENT (PRELIMINARY TEST)

Starting at 275°C, the weight of the sample decreased slightly, yet up to 550°C a significant decrease in sample weight was not observed.

After the experiment, a black molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test item. 

DSC EXPERIMENT 1

An endothermic peak was observed between 250°C and 275°C directly followed by exothermic effects starting at 275°C. The extrapolated onset temperature of the endothermic peak was 265.268°C. The endothermic effect was most likely caused by melting of the test item. The exothermic effects were ascribed to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was concluded that the test item had molten and that the change of the colour demonstrated 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 peak. The extrapolated onset temperature was 262.559°C. After the experiment, an off-white/yellowish molten residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test item. It also demonstrated that melting was the reason for the endothermic effect.

DSC EXPERIMENT 3

Since the difference in extrapolated onsets between the first two experiments was > 1°C, Experiment 3 was performed using the same conditions as in Experiment 2. The extrapolated onset of the melting peak was 263.042°C. After the experiment, an off-white/yellowish molten residue remained in the sample container.

DATA HANDLING

Since reaction and/or decomposition was observed during melting of the test item, a relatively high difference between the extrapolated onsets was observed. Therefore a melting range was given instead of a melting temperature. The melting range was determined between the lowest and highest melting temperature of Experiment 1 (265.268°C), Experiment 2 (262.559°C) and Experiment 3 (263.042°C).

Applicant's summary and conclusion

Conclusions:
The melting range of the substance was determined to be 262.6-265.3°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.

A melting range instead of a well defined melting temperature was determined. The melting range of the substance was determined to be 262.6-265.3°C.

Reaction and/or decomposition of the substance started during melting.