4-Piperidinecarboxylic acid, hydrochloride (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:

26 August - 22 December 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

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

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

4-piperidinecarboxylic acid hydrochloride

EC Number:

611-901-9

Cas Number:

5984-56-5

Molecular formula:

C6H11NO2.HCl

IUPAC Name:

4-piperidinecarboxylic acid hydrochloride

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-150098-AAC (T001310)
- Physical state: solid
- Appearance white powder

Specific details on test material used for the study:

- Batch n°: I14KB4913
- Analytical purity: 97.4% (base titration)
- Expiration date: 23 November 2020 (retest date)
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

298.2 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

Reaction and/or decomposition was observed directly after melting. A dark brown molten residue remained after the preliminary test and the main tests (original colour: white).

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 starting at 300°C. At 357°C the sample weight has decreased by 25%. After the experiment, a dark brown molten residue remained in the sample container (original colour: white) and a brown residue was observed on the lid of the sample container. The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

The DSC curve from the first experiment with a heating rate of 20°C/min showed a small endothermic peak between 150°C and 200°C. The extrapolated onset temperature of the peak was 184.08°C. According to information supplied by the sponsor, the effect was most likely obtained due to a solid-solid or phase transformation. A second endothermic peak was observed starting at 250°C. The extrapolated onset temperature of the peak was 298.20°C. This effect was most likely obtained due to melting followed by reaction and/or decomposition of the test item. After the experiment, a brown molten residue remained. To investigate the endothermic peak between 150°C and 200°C, a repeated heating cycle was applied in Experiment 2. The extrapolated onset temperature of the peak was 184.29°C. After the experiment the material seemed unchanged. Experiment 3 was performed to investigate the endothermic peak starting at 250°C. The extrapolated onset temperature of the first peak was 184.31°C and of the second peak 298.26°C. After the experiment, a white molten residue remained in the sample container. The result demonstrated that the second endothermic effect was due to melting of the test item.

To further investigate the endothermic peak between 150°C and 200°C, a repeated heating cycle was applied in Experiment 4. The extrapolated onset temperature of the peak was 183.97°C. This peak can be related to a solid-solid or phase transformation.

The melting temperature of T001310 was determined as the average melting temperature obtained from Experiment 1 and Experiment 3 and equals 298.2°C (571.4K).

According to the sponsor, the second endothermic effect observed in Experiment 1 (184.08°C), Experiment 2 (184.29°C), Experiment 3 (184.31°C) and Experiment 4 (183.97°C), derives from a

solid-solid or phase transformation.

Applicant's summary and conclusion

Conclusions:

JNJ-150098-AAC (T001310) was determined to be 298.2°C (571.4K) by using DSC.
According to the sponsor, a second endothermic effect observed at 184.2°C (457.3K), derives from a solid-solid or phase transformation.
Reaction and/or decomposition of the test item was observed directly after melting.