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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
20 February - 22 March 2018
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:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry

Test material

Constituent 1
Chemical structure
Reference substance name:
(2S,3S)-3-(ethoxycarbonyl)bicyclo[2.2.2]octan-2-aminium chloride
Cas Number:
1626394-43-1
Molecular formula:
C11H19NO2.HCl
IUPAC Name:
(2S,3S)-3-(ethoxycarbonyl)bicyclo[2.2.2]octan-2-aminium chloride
Test material form:
solid: particulate/powder
Details on test material:
- Physical state: powder
- Appearance: white powder
Specific details on test material used for the study:
- Batch n°: M16HD2757
- Analytical purity: 95.1% (determined by GC assay)
- Expiration date: 04 July 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
148.6 °C
Atm. press.:
1 013.25 hPa
Decomposition:
yes
Decomp. temp.:
> 200 °C
Remarks on result:
other: A yellow and off-white molten residue remained after the preliminary and first main test, respectively, indicating reaction and/or decomposition.

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 250°C. At 259°C the sample weight has decreased by 25%. After the experiment, a yellow molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 100°C and 175°C. The extrapolated onset temperature of the peak was 148.597°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 200°C due to reaction and/or decomposition of the test item. After the experiment, an off-white molten residue remained. To investigate the melting peak between 100°C and 175°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 148.674°C. The melting temperature of T003680 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 148.6°C (421.8K).

Applicant's summary and conclusion

Conclusions:
The melting temperature of JNJ-63756992-AAC (T003680) was determined at 148.6°C (421.8K) by using DSC.