1-(6-FLUORO-3,4-DIHYDRO-2H-CHROMEN-2-YL)ETHANONE

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

29 June 2016 - 29 November 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:

1-(6-fluoro-3,4-dihydro-2H-1-benzopyran-2-yl)ethan-1-one

Cas Number:

620176-90-1

Molecular formula:

C11H11FO2

IUPAC Name:

1-(6-fluoro-3,4-dihydro-2H-1-benzopyran-2-yl)ethan-1-one

Test material form:

liquid

Details on test material:

- Name of test material (as cited in study reports): JNJ-7928531-AAA (T001481)
- Physical state: liquid
- Appearance: Colourless, light yellow to brown liquid

Specific details on test material used for the study:

- Batch n°: M16AB0419
- Expiration date: 23 September 2016
- Purity: 102.5% (based on GC assay)
- Storage condition of test material: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

-65.5 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 175 °C

Remarks on result:

other: During the test no melting was observed.

Remarks:

Glass transition temperature is reported

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 175°C. At 265°C the sample weight has decreased by 25%.

After the experiment it was observed that the test item was evaporated from the sample container.

Main tests

During cooling a glass transition was observed between -85°C and -60°C. During heating a glass transition between -75°C and -50°C was observed. The inflection point of the glass transition was -65.417°C. An endothermic peak between 200°C and 300°C was observed. The extrapolated onset temperature of the peak was 276.807°C. The effect was most likely obtained due to boiling of the test item. After the experiment it was observed that the test item was evaporated from the sample container.

Experiment 2 was performed to investigate the boiling point and is explained in the next section.

Experiment 3 was performed to investigate reaction and/or decomposition of the test item and was therefore

stopped at 280°C. At approximately 110°C a small signal was observed: it was most likely an artefact. From 175°C the baseline deviated in the endothermic direction. After the experiment, a light yellow residue remained in the sample container which demonstrated that reaction and/or decomposition of the test item probably took place over the temperature range.

The glass transition temperature was determined as the average glass transition temperature obtained from experiment 1 (-65.417°C) and experiment 2 (-65.586°C). No melting was observed.

Applicant's summary and conclusion

Conclusions:

The glass transition temperature of JNJ-7928531-AAA (T001481) was determined at -65.5°C (207.6K) by using DSC.