1-benzyl-4-piperidone

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 February 2017 - 12 May 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

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:

1-benzyl-4-piperidone

EC Number:

222-782-4

EC Name:

1-benzyl-4-piperidone

Cas Number:

3612-20-2

Molecular formula:

C12H15NO

IUPAC Name:

1-benzylpiperidin-4-one

Test material form:

liquid

Details on test material:

- Identification: JNJ-728195-AAA
- Physical state: liquid
- Appearance: clear yellowish liquid

Specific details on test material used for the study:

- Batch n°: I15EB2027
- Analytical purity: 99.6% (based on base titration)
- Expiration date: 2017-07-25
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 150 °C

Remarks on result:

other: The glass transition temperature was determined to be -65.4°C (207.8K)

Remarks:

An orange/red residue and a light brown/orange residue remained after the preliminary and 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 200°C. At 281°C the sample weight has decreased by 25%. After the experiment, a orange/red residue remained in the sample container (original colour: yellowish). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

During cooling a glass transition was observed between -90°C and -60°C (results are archived in the raw data). During heating a glass transition between -75°C and -50°C was observed. The inflection point of the glass transition was -65.272°C. An endothermic peak started from 150°C. The effect was due to reaction and/or decomposition of the test item. After the experiment, a light brown/orange residue remained in the sample container.

Experiment 2 was performed to determine the duplicate melting temperature of the test item. The temperature program was similar as of Experiment 1 as well as the results were similar. The inflection point of the glass transition was -65.453°C. After the experiment, a light brown/orange residue remained in the sample container.

The glass transition temperature was determined as the average glass transition temperature obtained from Experiment 1 (-65.272°C) and Experiment 2 (-65.453°C).

Applicant's summary and conclusion

Conclusions:

The glass transition temperature of JNJ-728195-AAA (T000015) was determined to be -65.4°C (207.8K) using DSC.