1H-Pyrazolo[3,4-b]pyridine-3-carboximidamide, 5-fluoro-1-[(2-fluorophenyl)methyl]-

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

May 21, 2019 to June 04, 2019

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Boiling pt.:

> 290 °C

Atm. press.:

ca. 1 000 hPa

Decomposition:

yes

Decomp. temp.:

> 290 °C

Boiling point / boiling range: DSC measurement

One DSC measurement in an aluminium crucible with a hole showed an endothermal effect after the melting in the temperature range of 290 – 340 °C, directly followed by an exothermal effect in the temperature range of 340 – 360 °C.

No further endothermal or exothermal effects were observed up to the final temperature of 500 °C. After the DSC measurement the test item was a black residue and a mass loss 76 % was observed.

The onset temperature (see Table 2) was derived from the intersection of the tangent line with the highest slope of the endothermal peak with the baseline. The results of the DSC measurement are summarized in Table 2.

Table 2: Boiling point (DSC measurement)

Ident No.	Test item /mg	Starting temperature /°C	Final test temperature /°C	Temperature range (endothermal) /°C	Onset  (boiling) /°C	Crucible	Observations after the measurement
38673	13.55	25	500	290 – 340	multistage	Aluminium with a hole	Test item discoloured into black

                        

Boiling point / boiling range: Capillary tube in a metal block

A measurement with the capillary method was performed to clarify the results of the DSC measurements. Since this measurement was performed only as a verifying screening a high heating rate of 10 K/min was chosen and therefore the absolute temperature values derived with the capillary method are not as accurate as the DSC results. The filling height of the test item was approximately 5 mm. The results are summarized in Table 3.

Table 3: Results of the capillary method

No.	Set point /°C	Heating rate / K/min	Endpoint /°C	Remarks
1	250	10	380	250 °C: Test item appeared as a slightly orange turbid melt 272 °C: Test item appeared as a slightly orange clear melt 305 °C: Test item started bubble formation 322 °C: Test item boiled and got darker coloured (amber) 336 °C: Test item stopped boiling and appeared as a brown solid at the surface of the capillary 363 °C: The brown solid melted under formations of small gas bubbles 380 °C: no further change

                        

                       

Under consideration of the results from the DSC measurements and the capillary method it was concluded that the test item boiled under decomposition starting at approx. 290 °C.

Executive summary:

The test item boiled under decomposition starting at approx. 290 °C.

Description of key information

The test item boiled under decomposition starting at approx. 290 °C.

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