2-Propenamide, N-[5-[[4-[4-[(dimethylamino)methyl]-3-phenyl-1H-pyrazol-1-yl]-2-pyrimidinyl]amino]-4-methoxy-2-(4-morpholinyl)phenyl]

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

05 Oct 2020 to 04 Dec 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Cross-reference

Reason / purpose for cross-reference:

reference to same study

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

05 Oct 2020 to 04 Dec 2020

Reliability:

1 (reliable without restriction)

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- lot/batch number of test material: M20BD0542
- Expiry date: 19 February 2022 (retest date)
- Physical Description: Slightly greenish yellow powder
- Purity: 99.8%
- Purity correction factor: 1.00

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Final preparation of a solid: not applicable, the solid test item was transferred directly into the DSC cell

Key result

Decomposition:

yes

Decomp. temp.:

225 °C

Remarks on result:

other: Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.

Preliminary test

From the TGA curve it could be derived that starting at 300 °C the weight of the sample decreased significantly. At 398°C, the sample weight had decreased by 25%.
After the experiment, a black charred residue remained in the sample container (original colour: slightly greenish yellow). The change of the colour indicated reaction  and/or decomposition of the test item.

 

Main test

From the DSC curve obtained with experiment 2, an endothermic effect was observed between 175°C and 225°C directly followed by an exothermic effect starting at 225°C. The extrapolated onset temperature of the endothermic effect was 221.010°C. This effect was most likely obtained due to melting of the test item. The exothermic effect was probably obtained due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained in the sample container (original colour: slightly greenish yellow). The change of the colour indicated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, Experiment 3 was stopped directly after the melting effect.The extrapolated onset temperature was 221.175°C. After the experiment, a yellow molten residue remained in the sample container (original colour: slightly greenish yellow). It demonstrated that melting was the reason for the endothermic effect.

Reaction and/or decomposition of the test item was observed during DSC experiment starting at 225°C (494.2K). Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.

Conclusions:

Boiling of the test item was not observed below the temperature at which reaction and/or
decomposition started. Based on this, the test item has no boiling temperature.

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:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

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:

N-{5-[(4-{4-[(dimethylamino)methyl]-3-phenyl-1H-pyrazol-1-yl}pyrimidin-2-yl)amino]-4-methoxy-2-(morpholin-4-yl)phenyl}prop-2-enamide

EC Number:

841-500-6

Cas Number:

1903008-80-9

Molecular formula:

C30H34N8O3

IUPAC Name:

N-{5-[(4-{4-[(dimethylamino)methyl]-3-phenyl-1H-pyrazol-1-yl}pyrimidin-2-yl)amino]-4-methoxy-2-(morpholin-4-yl)phenyl}prop-2-enamide

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- lot/batch number of test material: M20BD0542
- Expiry date: 19 February 2022 (retest date)
- Physical Description: Slightly greenish yellow powder
- Purity: 99.8%
- Purity correction factor: 1.00

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Final preparation of a solid: not applicable, the solid test item was transferred directly into the DSC cell

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

221.1 °C

Decomposition:

yes

Decomp. temp.:

225 °C

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that starting at 300 °C the weight of the sample decreased significantly. At 398°C, the sample weight had decreased by 25%.
After the experiment, a black charred residue remained in the sample container (original colour: slightly greenish yellow). The change of the colour indicated reaction  and/or decomposition of the test item.

 

Main test

From the DSC curve obtained with experiment 2, an endothermic effect was observed between 175°C and 225°C directly followed by an exothermic effect starting at 225°C. The extrapolated onset temperature of the endothermic effect was 221.010°C. This effect was most likely obtained due to melting of the test item. The exothermic effect was probably obtained due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained in the sample container (original colour: slightly greenish yellow). The change of the colour indicated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, Experiment 3 was stopped directly after the melting effect.The extrapolated onset temperature was 221.175°C. After the experiment, a yellow molten residue remained in the sample container (original colour: slightly greenish yellow). It demonstrated that melting was the reason for the endothermic effect.
The melting temperature was determined as the mean melting temperature of Experiment 2 (221.010°C) and Experiment 3 (221.175°C). 

Applicant's summary and conclusion

Conclusions:

The melting and boiling temperature of JNJ-73841937-AAA (T003925) were determined by DSC.
The melting temperature of the test item was 221.1°C (494.2K).
Reaction and/or decomposition of the test item was observed during DSC experiment starting at 225°C (494.2K).
Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature.