3-bromo-5-fluoro-1-[(4-methylphenyl)sulfonyl]-1H-pyrrolo[2,3-b]pyridine

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

29 January - 22 March 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

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:

3-bromo-5-fluoro-1-(4-methylbenzenesulfonyl)-1H-pyrrolo[2,3-b]pyridine

Cas Number:

1417421-99-8

Molecular formula:

C14H10BrFN2O2S

IUPAC Name:

3-bromo-5-fluoro-1-(4-methylbenzenesulfonyl)-1H-pyrrolo[2,3-b]pyridine

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

- Batch n°: I16FD3006
- Analytical purity: 100.1%
- Expiration date: 16 June 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

162.4 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 275 °C

Remarks on result:

other: A black expanded residue and a dark red/brown/black molten residue remained after the preliminary and main test 1, indicating reaction and/or decomposition.

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 300°C. At 306°C the sample weight has decreased by 25%. After the experiment, a black 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 between 150°C and 200°C. The extrapolated onset temperature of the peak was 162.347°C. The effect was most likely obtained due to melting. An exothermic peak was observed starting at 275°C. After the experiment, a dark red/brown/black molten residue remained. To investigate the endothermic peak, a repeated heating cycle was applied and stopped at 180°C. The extrapolated onset temperature of the melting peak was 162.434°C. The melting temperature was determined as the average melting temperature obtained from experiment 1 and experiment 2 and equals162.4°C (435.5K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-63757031-AAA (T003685) was determined at 162.4°C (435.5K) by using DSC.
Reaction and/or decomposition was observed during DSC at temperatures of > 275°C (>548K).