4-(p-chlorophenyl)piperidin-4-ol

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

08 March - 11 October 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:

4-(p-chlorophenyl)piperidin-4-ol

EC Number:

254-479-8

EC Name:

4-(p-chlorophenyl)piperidin-4-ol

Cas Number:

39512-49-7

Molecular formula:

C11H14ClNO

IUPAC Name:

4-(p-chlorophenyl)piperidin-4-ol

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-117676-AAA (T000263)
- Physical state: solid (powder)
- Appearance: White, slight beige amorphous, crystalline, micropowder

Specific details on test material used for the study:

- Batch n°: I15BB0491
- Analytical purity: 99.8% (base titration)
- Expiration date: 04 February 2021
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

140 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A brown molten residue remained after the preliminary test and a yellow molten residue remained after the main test (up to 311°C), indicating reaction and/or decomposition.

Decomp. temp.:

> 250 °C

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 275°C. At 311°C the sample weight has decreased by 25%. After the experiment, a brown molten residue remained in the sample container (original colour: white to slightly grey powder). 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 an endothermic peak between 125°C and 150°C. The extrapolated onset temperature of the peak was 139.97°C. The effect was most likely obtained due to melting.

From 250°C a small exothermic followed by an endothermic effect was observed. The effect was most likely due to the start of reaction and/or decomposition of the test item. After the experiment, a yellow molten residue remained.

To investigate the melting peak between 125°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 139.93°C. The melting temperature of T000263 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 140.0°C (413.1K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-117676-AAA (T000263) was determined at 140.0°C (413.1K) by using DSC.