(1S)-2-(benzylamino)-1-[(2R)-6-fluoro-3,4-dihydro-2H-chromen-2-yl]ethanol

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

08 February 2016 - 11 July 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

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:

(1S)-2-(benzylamino)-1-[(2R)-6-fluoro-3,4-dihydro-2H-chromen-2-yl]ethanol

EC Number:

603-316-2

Cas Number:

129050-27-7

Molecular formula:

C18H20FNO2

IUPAC Name:

(1S)-2-(benzylamino)-1-[(2R)-6-fluoro-3,4-dihydro-2H-chromen-2-yl]ethanol

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-17298957-AAA (T001592)
- Physical state: solid (powder)
- Appearance: White powder

Specific details on test material used for the study:

- Batch n°: I15HB2929
- Analytical purity: 100% (Based on base titration assay)
- Expiration date: 14 Aug 2017
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

116.2 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A beige molten residue remained in the sample container due to reaction and/or decomposition.

Decomp. temp.:

> 250 °C

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 250°C. At 314°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 100°C and 150°C. The extrapolated onset temperature of the peak was 116.130°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 250°C due to reaction and/or decomposition of the test item. After the experiment, a beige molten residue remained. To investigate the melting peak between 100°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 116.189°C. The melting temperature of T001592 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 116.2°C (389.3K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-17298957-AAA (T001592) was determined at 116.2°C (389.3K) by using DSC.