4-[(4-HYDROXYPYRIMIDIN-2-YL)AMINO]BENZONITRILE

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 assesment.

GLP compliance:

not specified

Type of method:

thermal analysis

Melting / freezing pt.:

ca. 300 °C

Decomposition:

yes

Decomp. temp.:

ca. 300 °C

Conclusions:

The melting point of T002487was determined to be ca. 300°C. Decomposition was observed at ca. 300°C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

09 March - 21 July 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°: M15GC2731
- Analytical purity: 99.8%
- Expiration date: 23 July 2016
- Storage condition: at room temperature protected from light

Key result

Melting / freezing pt.:

322.8 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

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

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly from 320°C. At 384°C the sample weight has decreased by 25%. After the experiment, a black 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 was obtained and showed an endothermic peak from 300°C. The extrapolated onset temperature of the peak was 322.78°C. The effect was most likely obtained due to melting. After the experiment, a brown molten residue remained. The change of the colour demonstrated reaction and/or decomposition of the test item.

To investigate the melting peak from 300°C, a repeated heating cycle was applied and stopped directly after melting. The extrapolated onset temperature of the melting peak was 322.76°C. After the experiment, an orange molten residue remained.The change of the colour demonstrated reaction and/or decomposition of the test item.

The melting temperature of T002487 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 322.8°C (596K).

Conclusions:

The melting temperature of JNJ-40370226-AAA (T002487) was determined at 322.8°C (596K) 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, Ciric, 2016) the melting point of T002487 was determined to be 322.8°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

322.8 °C

Additional information

A supporting study (Janssen Pharmaceutica Process Safety Center, 2013) with insufficient documentation, and therefore assigned as Klimisch 4 study, concluded that the melting temperature of T002487 is about 300°C, which is in line with the result of the key study by Ciric (2016).