Formamide, N-[(2-bromo-5-hydroxy-4-methoxyphenyl)methyl]-N-[2-(4-hydroxyphenyl)ethyl]-

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

Reliability:

4 (not assignable)

Rationale for reliability incl. deficiencies:

other: Documentation insufficient for assessment. No information on purity of the substance.

GLP compliance:

not specified

Type of method:

thermal analysis

Melting / freezing pt.:

ca. 165 °C

It is the result of either thermal analysis in DSC apparatus on mg scale and/or other DTA equipment (Differentrial Temperature Analysis ) on gram scale.

Conclusions:

The melting point of the T002078 is ca. 165 deg C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-01-12 to 2017-04-25

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°: I15EB1917
- Analytical purity: 98.9%
- Expiration date: 2017-09-07
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

162.3 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

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

Decomp. temp.:

>= 250

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 275°C. At 332°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: white, brown grey). 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 was obtained and showed an endothermic peak between 150°C and 200°C. The extrapolated onset temperature of the peak was 162.3°C. The effect was most likely obtained due to melting. A second endothermic peak was observed between 250°C and 325°C due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained. To investigate the melting peak between 150°C and 200°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 162.27°C. The melting temperature of T002078 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 162.3°C (523K).

Conclusions:

The melting temperature of JNJ-28645409-AAA (T002078) was determined at 162.3°C (435.4K) 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, 2017) the melting point of T002078 was determined to be 162.3°C (435.4K).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

162.3 °C

Additional information

A supporting study (Janssen Pharmaceutica Process Safety Center, 1996) with insufficient documentation, and therefore assigned as Klimisch 4 study, concluded that the melting temperature of T002078 is about 165°C, which is in line with the result of the key study by Brekelmans (2017).