N-phenyl-N-piperidin-4-ylpropionamide

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

10 November 2015 - 24 May 2016

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 (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

N-phenyl-N-piperidin-4-ylpropionamide

EC Number:

216-543-3

EC Name:

N-phenyl-N-piperidin-4-ylpropionamide

Cas Number:

1609-66-1

Molecular formula:

C14H20N2O

IUPAC Name:

N-phenyl-N-piperidin-4-ylpropionamide

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-1594255-AAA (T000425)
- Physical state: solid (powder)
- Appearance: white

Specific details on test material used for the study:

- Batch n°: I15KB4578
- Analytical purity: 99.3% (base titration)
- Expiration date: 26 November 2017
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

91.8 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 250 °C

Remarks on result:

other: A dark brown molten residue remained after the preliminary test and a colourless molten residue remained after the 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 250°C. At 302°C the sample weight has decreased by 25%. After the experiment, a dark brown 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 showed a small endothermic peak between 50°C and 75°C and a major endothermic peak between 75°C and 125°C were observed. The small peak might have been due to melting of an impurity. The extrapolated onset temperature of the major peak was 91.627°C. The effect was most likely obtained due to melting of the test item. Furthermore, a very slight deviation from the baseline in endothermic direction was observed from 250°C. This signal was most probably – especially in view of the weight loss and colour change of the test item during the preliminary test – due to reaction and/or decomposition of the test item. After the experiment, a colourless molten residue remained in the sample container. To investigate the melting peak between 75°C and 125°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 92.041°C. The melting temperature of T000425 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 91.8°C (365.0K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-1594255-AAA (T000425) was determined at 91.8°C (365.0K) using DSC.