4-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2021-01-12 to 2021-03-01

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2021

Report date:

2021

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

March 1998

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

July 27, 1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

March 04, 2016

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-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Cas Number:

2270944-70-0

Molecular formula:

C15H16ClN5O4

IUPAC Name:

4-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Batch (Lot) Number: I20CD1048
- Purity/Composition: 100%
- Purity test date : 2020-05-11
- Expiry date: 2022-03-22 (retest date)
- Physical Description: Light yellow to dark orange solid

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability and homogeneity of the test material in the vehicle/solvent under test conditions and during storage: not indicated
- Stability in the medium, i.e. sensitivity of the test material to hydrolysis and/or photolysis: not indicated
- Solubility and stability of the test material in the solvent/vehicle and the exposure medium: not indicated
- Reactivity of the test material with the incubation material used (e.g. plastic ware): not indicated

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
No treatment

OTHER SPECIFICS
- Purity/Composition correction factor: Yes, correction factor is 1.0

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

195.7 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

225 °C

Any other information on results incl. tables

Preliminary Test
Starting at 200°C, the weight of the sample decreased significantly. At 374°C, the sample weight had decreased by 25%. After the experiment, a black charred residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item.

Main Study
In experiment 1, an endothermic effect directly followed by a strong exothermic was observed between 175°C and 225°C. The extrapolated onset temperature of the endo effect was 195.675°C. These effects were most likely obtained due to melting directly followed by reaction and/or decomposition of the test item.

After the experiment, a black charred residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item. In order to investigate the endothermic effect, Experiment 2 was stopped directly after the melting effect. The extrapolated onset temperature was not determined since there is no entire peak showed. After the experiment, a black molten residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, a higher end temperature was used in the Experiment 3. The extrapolated onset temperature was 195.787°C. After the experiment, a black molten residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

The melting temperature was determined as the mean melting temperature of Experiment 1 (195.675°C) and Experiment 3 (195.787°C).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-73848242-AAA (T003901) was determined by DSC.
The melting temperature of the test item was 195.7°C (468.9K).
Reaction and/or decomposition of the test item were observed during DSC experiments
during melting and directly after melting.