2H-1-Benzopyran, 6-fluoro-3,4-dihydro-2-[(2S)-2-oxiranyl]-, (2R)-

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

20 February 2017 to 02 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:

(2R)-6-fluoro-2-[(2S)-oxiran-2-yl]-3,4-dihydro-2H-1-benzopyran

EC Number:

603-315-7

Cas Number:

129050-26-6

Molecular formula:

C11H11FO2

IUPAC Name:

(2R)-6-fluoro-2-[(2S)-oxiran-2-yl]-3,4-dihydro-2H-1-benzopyran

Test material form:

other: wax

Details on test material:

Physical state: wax form
Appearance: clear, viscous, wax

Specific details on test material used for the study:

- Batch n°: I16HB3199
- Analytical purity: 98.9%
- Expiration date: 2017-09-13 (retest date)
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

43.8 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 150 °C

Remarks on result:

other: A brown orange molten residue remained after the preliminary test, and a colourless molten residue remained after the 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 220°C. At 268°C the sample weight has decreased by 25%. After the experiment, a brown orange molten residue remained in the sample container (original colour: pale yellow). 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 0°C and 75°C. The extrapolated onset temperature of the peak was 41.984°C. The effect was most likely obtained due to melting of the test item. From 150°C a second endothermic effect was observed. After the experiment, a yellow (darker then original) residue remained in the sample container. The effect was, therefore, considered due to reaction and/or decomposition.

To investigate the melting peak, the temperature program of the second experiment was stopped after the endothermic effect. The extrapolated onset temperature of the melting peak was 43.709°C. After the experiment, a colourless molten residue remained in the sample container.

The difference in the extrapolated onset of the melting peak between Experiment 1 and Experiment 2 was > 0.5°C. Therefore Experiment 3 was performed. The temperature program was identical to Experiment 2. The extrapolated onset of the melting peak was 43.799°C. After the experiment, a colourless molten residue remained in the sample container.

 

The melting temperature was determined as the average melting temperature obtained from Experiment 2 (43.709°C) and Experiment 3 (43.799°C). The first extrapolated onset temperature was not taken into account for the calculation of the melting temperature, as it deviated more than 0.5°C from the onset temperature of Experiment 2 and 3.

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-17337359-AAA (T001590) was determined at 43.8°C (316.9K) using DSC.