2-(4-fluorophenyl)-5-(5-iodo-2-methylbenzyl)thiophene

Melting point / freezing point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

2008

Reliability:

4 (not assignable)

Rationale for reliability incl. deficiencies:

documentation insufficient for assessment

Qualifier:

no guideline followed

Principles of method if other than guideline:

Approximate figure based on thermal analysis runs performed for safety reasons (thermal stability) by the Process Safety Center.
It is the result of either thermal analysis in DSC apparatus on mg scale and/or other DTA equipment (Differential Temperature Analysis) on gram scale.

GLP compliance:

no

Type of method:

thermal analysis

Melting / freezing pt.:

109 °C

Decomposition:

yes

Decomp. temp.:

>= 300 °C

Conclusions:

T003063 has a melting point of about 109°C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

26 September 2015 - 21 January 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

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

Specific details on test material used for the study:

- Batch n°: M14KB4863
- Analytical purity: 100.5% (based on assay)
- Expiration date: 10 November 2017 (retest date)
- Storage condition: At room temperature

Key result

Melting / freezing pt.:

109.4 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A black molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.

Decomp. temp.:

300 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 350°C. At 365°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: white to almost white). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

The DSC curve with a heating rate of 20°C/min showed an endothermic peak between 100°C and 150°C. The extrapolated onset temperature of the peak was 109.33°C. The effect was most likely obtained due to melting. After the experiment, a yellow/brown molten residue remained. To investigate the melting peak between 100°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 109.37°C. After the experiment, a black molten residue remained in the sample container caused by reaction and/or decomposition. The melting temperature of T003063 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 109.4°C (382.5 K).

Conclusions:

The melting temperature of JNJ-39453193-AAA (T003063) was determined at 109.4°C (382.5 K) by using DSC.

Description of key information

In a GLP study according to OECD guideline 102, EU method A.1 and EPA OPPTS 830.7200 (Klimisch 1, Brekelmans, 2016) the melting point of T003063 was determined to be 109.4°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

109.4 °C

Additional information

A supporting study (Janssen Pharmaceutica Process Safety Center, 2008) with insufficient documentation, and therefore assigned as Klimisch 4 study, concluded that the melting temperature of T003063 is about 109°C, which is in line with the result of the key study by Brekelmans (2016).