(2R)-6-fluoro-2-(oxiran-2-yl)chromane

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

07 March - 17 September 2017

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:

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

Remarks:

glass transition temperature

Test material

Test material information

Constituent 1

Reference substance name:

(2R)-6-fluoro-2-(oxiran-2-yl)chromane

EC Number:

930-890-4

Cas Number:

1219915-04-4

Molecular formula:

C11H11FO2

IUPAC Name:

(2R)-6-fluoro-2-(oxiran-2-yl)chromane

Test material form:

liquid

Details on test material:

- Name of test material (as cited in study reports): JNJ-42398681-AAA (T001589)
- Physical state: liquid
- Appearence: light brown

Specific details on test material used for the study:

- Batch n°: I16FB3011
- Analytical purity: 87%
- Expiration date: 14 March 2018
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 150 °C

Remarks on result:

other: the glass transition temperature was determined to be -52.1°C

Remarks:

An orange residue remained after the preliminary and the first 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 from 225°C upwards. At 279°C the sample weight has decreased by 25%. After the experiment, a orange 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

In order to determine the melting more precisely, the DSC curve was obtained and showed a glass transition temperature (T_G) between -50°C and -80°C during cooling. During heating a glass transition of the test item was observed between -75°C and -25°C. The inflection point was -52.044°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, an orange residue remained in the sample container.

 

Experiment 2 was performed to determine the duplicate inflection point of the T_G. The temperature program of the second experiment was stopped after the glass transition. The inflection point of the glass transition was -52.243°C. After the experiment, the residue in the sample container remained unchanged.

 

The T_Gwas determined as the average temperature obtained from Experiment 1 (-52.044°C) and Experiment 2 (-52.243°C).

Applicant's summary and conclusion

Conclusions:

The glass transition temperature of JNJ-42398681-AAA (T001589) was determined at -52.1°C (221.0K) by using DSC. No melting was observed.