ethyl (2S,3S)-3-[(2-chloro-5-fluoro-4-pyrimidinyl)amino]bicyclo[2.2.2]octane-2-carboxylate

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

30 January 2018 - 20 April 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:

ethyl (2S)-3-[(2-chloro-5-fluoropyrimidin-4-yl)amino]bicyclo[2.2.2]octane-2-carboxylate

EC Number:

821-183-0

Cas Number:

1777721-57-9

Molecular formula:

C15H19ClFN3O2

IUPAC Name:

ethyl (2S)-3-[(2-chloro-5-fluoropyrimidin-4-yl)amino]bicyclo[2.2.2]octane-2-carboxylate

Test material form:

solid: particulate/powder

Details on test material:

Physical state: solid
Appearance: White powder

Specific details on test material used for the study:

- Batch n°: I16DD2146
- Analytical purity: 99.7% (based on GC assay)
- Expiration date: 27 April 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

ca. 129.5 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 250 °C

Remarks on result:

other: A a black charred residue remained after the preliminary and main test, 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 325°C. At 334°C the sample weight has decreased by 25%. After the experiment, a black charred 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 150°C. The extrapolated onset temperature of the peak was 129.647°C. The effect was most likely obtained due to melting. After the experiment, a a brown molten residue remained. In order to investigate the endothermic peak,a second experiement was stopped directly after the melting peak. The extrapolated onset temperature of the melting peak was 129.403°C. The melting temperature of T003688 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 129.5°C (406.7K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-63757083-AAA (T003688) was determined at 129.5°C (406.7K) by using DSC.