(R)-2-(2,5-difluorophenyl)pyrrolidine (R)-2-hydroxysuccinate

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

27 May 2021

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

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

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

ca. 87 °C

Any other information on results incl. tables

Melting point / melting range: DSC measurement
Two DSC measurements with a heating rate of 10 K/min and a final temperature of 500 °C showed an endothermal effect (melting) in the temperature range of 70 – 100 °C. At approximately 100 °C exothermal effects started. After the DSC measurements black residues were observed and a mass loss of 87%.

In the third DSC measurement with a heating rate of 10 K/min and a final temperature of 100 °C showed an endothermal effect (melting) in the temperature range of 75 – 100 °C. After the DSC measurements the test was a clear melt and no mass loss was observed.

The onset temperature (see Table 1) 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 measurements are summarized in Table 1.

ID	test item [mg]	start temperature [°C]	final temperature [°C]	temperature range [°C	onset [°C]	crucible	observations after measurement
1	12.72	25	500	70 - 100	86.69	aluminium with a hole	black residue, mass loss 87%
2	10.12	25	500	70 - 95	84.68	aluminium with a hole	black residue, mass loss 87%
3	9.75	25	100	75 - 100	84.42	aluminium with a hole	clear melt, no mass loss

Applicant's summary and conclusion

Conclusions:

The test item had a melting range of 84 to 87 °C.

Executive summary:

Test Design: The melting point is determined by differential scanning calorimetry (DSC). The test item and the reference item are heated up from the starting temperature to the final temperature at a constant heating rate in a defined atmosphere (nitrogen). Open crucibles are used as containers for the test item and as empty reference crucible. The quantity of heat absorbed or released is measured and recorded.

Result: The test item had a melting range of 84 to 87 °C.