ethyl (2S,3S)-3-aminobicyclo[2.2.2]octane-2-carboxylate monohydrochloride

Melting point / freezing point

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 guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 3

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

Test material information

Constituent 1

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.