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

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

7 March - 16 September 2017

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

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

(2S)-6-fluoro-2-[(2S)-oxiran-2-yl]chromane [S-(R*,R*)]

EC Number:

603-314-1

Cas Number:

129050-23-3

Molecular formula:

C11H11FO2

IUPAC Name:

(2S)-6-fluoro-2-[(2S)-oxiran-2-yl]chromane [S-(R*,R*)]

Test material form:

liquid: viscous

Details on test material:

- Physical state: liquid (viscous)
- Appearance: clear viscous liquid

Specific details on test material used for the study:

- Batch n°: I16DB1991
- Analytical purity: 81.4 - 81.8%
- Expiration date: 7 June 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

-49.4 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A dark yellow to orange brown molten residue remained after the preliminary and main test, indicating reaction and/or decomposition.

Decomp. temp.:

> 150 °C

Remarks on result:

other: Glass transition temperature

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 225°C. At 288°C the sample weight has decreased by 25%. After the experiment, an orange brown molten residue remained in the sample container (original colour: yellow). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

During cooling a glass transition (TG) of the test item was observed between -40°C and -80°C. During heating a glass transition (TG) was observed between -75°C and -25°C. The inflection point was -49.530°C. Starting at 150°C, the DSC curve showed an endothermic effect. The effect was most likely due to the start of reaction and/or decomposition, based on the results obtained by the preliminary test and the change of colour. After the experiment, a dark yellow molten residue remained in the sample container.

 

Experiment 2 was performed to determine the duplicate inflection point of the glass transition (TG). The temperature program of the second experiment was stopped after the glass transition. The inflection point of the glass transition was -49.297°C. After the experiment, the residue remained in the sample container was unchanged.

 

The glass transition was determined as the average glass transition obtained from Experiment 1 (-49.530°C) and Experiment 2 (-49.297°C).

Applicant's summary and conclusion

Conclusions:

The glass transition temperature of JNJ-17337073-AAA (T001598) was determined at -49.4°C (223.7K) using DSC. No melting was observed.
Reaction and/or decomposition of JNJ-17337073-AAA (T001598) was observed during DSC experiment at temperatures of > 150°C (> 423K).