4-Bromo-2-fluoro-N-methylbenzamide

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 SEP 2022 TO 14 OCT 2022

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2022

Report date:

2022

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

November 2019

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

July 1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Version / remarks:

August 1996

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-Bromo-2-fluoro-N-methylbenzamide

EC Number:

808-257-8

Cas Number:

749927-69-3

Molecular formula:

C8H7BrFNO

IUPAC Name:

4-Bromo-2-fluoro-N-methylbenzamide

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: 21NN31395
- Expiry date: 18 December 2022 (retest date)
- Physical Description: Almost white powder
- Purity: 100.5%
- Purity test date: 25 JAN 2022
- Purity correction factor: 1.00
STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability under storage conditions: no data
- Stability under test conditions: no data
- Solubility and stability of the test item in the solvent/vehicle: no data
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

Boiling point

Key result

Boiling pt.:

>= 167.5 - <= 170 °C

Atm. press.:

1 011 hPa

Decomposition:

yes

Decomp. temp.:

275 °C

Remarks on result:

other: Evaporation of the sample occurred between 167.5°C and 170.0°C indicating a range of the evaporation temperature. This might indicate a potential boiling temperature.

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that starting at 175°C, the weight of the sample decreased significantly. At 252°C, the sample weight had decreased by 25%.

After the experiment it was observed that the test material was evaporated from the sample container (original colour: faint yellow. Observed colour in crucible: white).

Main study

During the Experiment 1, two endothermic effects were observed between 100°C and 150°C. An exothermic effect was observed between 275°C and 325°C. The first endothermic effect was obtained by unknown cause. The extrapolated onset temperature of the second effect was 125.199°C. The endothermic effect was most likely obtained due to melting of the test material. The exothermic effect was probably obtained due to reaction and/or decomposition of the test material. After the experiment it was observed that the test material had evaporated from the sample container.

To investigate the first endothermic effect, Experiment 2 was stopped after the first endothermic effect. After the experiment it was observed that the residue did not change from the original. The cause of the effect is unknown.

To investigate the second endothermic effect, Experiment 3 was stopped during the endothermic effect. After the experiment, a white molten residue remained in the sample container. It demonstrated that melting was the reason for the endothermic effect.

Experiment 4 was performed to investigate the residue before the exothermic effect. After the experiment it was observed that the test material had evaporated from the sample container.

Experiment 5 was performed to investigate the effects after the second endothermic effect. After the experiment a molten white residue remained in the sample container. It demonstrated that no effect occurred after the melting effect.

To investigate the exothermic effect, Experiment 6 was performed with a closed sample container and stopped after the exothermic effect. After the experiment a molten light brown residue remained in the sample container (observed appearance: white). The change of colour indicated reaction and/or decomposition of the test material.

Experiment 7 was performed with a golden sample container to investigate if a reaction occurred in the aluminium containers. After the experiment it was observed that there were no differences between measurements using an aluminium sample crucible or golden sample crucible.

No boiling temperature was found in experiments 2 to 6. Multiple measurements have been performed to distinguish the different events. From this it was concluded that no boiling point could be determined with DSC with evaluating an endothermic effect. Since evaporation of the test material did occur, an estimation of the evaporation temperature was performed by observing if test material still remained to recrystallise after heating above the melting temperature. Between the temperatures where recrystallisation occurs was the expected evaporation point.

Experiment 8 to 12 were performed consisting of a heating cycle, equilibration and cooling cycle to observe if a recrystallisation effect occurred. The results are presented in the table below. Recrystallization was observed between 90°C and 105°C.

DSC Experiments recrystallisation results

Experiment	9	10	11	12
End Temperature (°C)	150.0	170.0	165.0	167.5
Recrystallisation	Yes	No	Yes	Yes

It was observed that evaporation of the sample occurred between 167.5°C and 170.0°C indicating a range of the evaporation temperature.

Applicant's summary and conclusion

Conclusions:

The boiling temperature of JNJ-61789975-AAA (T003669) was determined by DSC.
Evaporation of the sample occurred between 167.5°C and 170.0°C indicating a range of the evaporation temperature. This might indicate a potential boiling temperature.
The atmospheric pressure was 1011 ± 3 hPa.
Reaction and/or decomposition of the test material was observed during DSC experiments starting at 275°C.