5-fluoro-1-[(4-methylphenyl)sulfonyl]-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-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:

25 January - 09 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:

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

EC Number:

812-520-2

Cas Number:

1259279-57-6

Molecular formula:

C20H22BFN2O4S

IUPAC Name:

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

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-63757044-AAA (T003686)
- Physical state: solid (powder)
- Appearance: white powder

Specific details on test material used for the study:

- Batch n°: I16HD3479
- Analytical purity: 100%
- Expiration date: 03 September 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

191.5 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 250 °C

Remarks on result:

other: A black and yellow molten residue remained after the preliminary and the first main test, respectively, and a colourless residue remained after the second main test, 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 325°C. At 343°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 between 175°C and 225°C. The extrapolated onset temperature of the peak was 191.499°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 250°C, probably due to reaction and/or decomposition of the test item. After the experiment, a yellow molten residue remained. The change of colour indicated reaction and/or decomposition of the test item.

To investigate the melting peak between 175°C and 225°C, a repeated heating cycle was applied which was stopped directly after the melting peak. The extrapolated onset temperature of the melting peak was 191.462°C. The melting temperature of T003686 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 191.5°C (464.6K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-63757044-AAA (T003686) was determined to be 191.5°C (464.6K) by using DSC.