Reaction mass of 6-butyl-3,6-dihydro-2,4-dimethyl-2H-pyran and 2-butyl-3,6-dihydro-4,6-dimethyl-2H-pyran and 2-butyltetrahydro-6-methyl-4-methylene-2H-pyran

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

05 January 2015 - 03 March 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2015

Report date:

2015

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

There were no deviations from standard operating procedures (SOPs).

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

There were no deviations from standard operating procedures (SOPs).

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

2-butyl-3,6-dihydro-4,6-dimethyl-2H-pyran

EC Number:

246-099-6

EC Name:

2-butyl-3,6-dihydro-4,6-dimethyl-2H-pyran

Cas Number:

24237-01-2

Molecular formula:

C11H20O

IUPAC Name:

2-butyl-4,6-dimethyl-3,6-dihydro-2H-pyran

Constituent 2

Reference substance name:

6-butyl-3,6-dihydro-2,4-dimethyl-2H-pyran

EC Number:

246-098-0

EC Name:

6-butyl-3,6-dihydro-2,4-dimethyl-2H-pyran

Cas Number:

24237-00-1

Molecular formula:

C11H20O

IUPAC Name:

6-butyl-2,4-dimethyl-3,6-dihydro-2H-pyran

Constituent 3

Reference substance name:

2-butyltetrahydro-6-methyl-4-methylene-2H-pyran

EC Number:

246-101-5

EC Name:

2-butyltetrahydro-6-methyl-4-methylene-2H-pyran

Cas Number:

24237-02-3

Molecular formula:

C11H20O

IUPAC Name:

2-butyl-6-methyl-4-methylenetetrahydro-2H-pyran

Specific details on test material used for the study:

Material Identification (as stated in the report) : Gyrane
Appearance: Colourless to pale yellow liquid
Batch: SC00008777

Please note that although the substance is described in the report with the IUPAC name: 6-Butyl-2,4-dimethyl-3,6-dihydro-2H-pyran related to the CAS number 24237-00-1, EC#246-098-0, recent analytical data had been determined the substance to be a multi-constituent described as Reaction mass of 6-butyl-3,6-dihydro-2,4-dimethyl-2H-pyran and 2-butyl-3,6-dihydro-4,6-dimethyl-2H-pyran and 2-butyltetrahydro-6-methyl-4-methylene-2H-pyran.
As the chemical manufacturing process has not changed since the report was written, the recent analytical information is relevant to the batch SC00008777 which was tested.

Results and discussion

Boiling point

Key result

Boiling pt.:

197 °C

Atm. press.:

1 026 hPa

Decomposition:

no

Any other information on results incl. tables

The DSC-curve is obtained with Experiment 1. During cooling, no effects were observed which were due to crystallization of the test substance (results are archived in the raw data). During heating, an endothermic peak between 150°C and 225°C was observed. The extrapolated onset temperature of the peak was 196.80°C.

The effect was most likely obtained due to evaporation of the test substance. After the experiment it was observed that no test substance was present in the sample container. To investigate the boiling peak between 150°C and 225°C a hermetic closed sample container was applied in Experiment 2. The extrapolated onset temperature of the evaporation peak was 200.60°C. As can be seen the endothermic peak shifted to higher temperatures. It demonstrated that evaporation of the test substance was the reason for the endothermic effect. Because the experiment was performed under higher pressure, the extrapolated onset temperature was not used for calculation of the boiling temperature.

After the experiment it was observed that no test substance was present in the sample container. Experiment 3 was performed to determine the duplicate boiling temperature of the test substance. The extrapolated onset of the evaporation peak was 196.79°C. After the experiment it was observed that no test substance was present in the sample container.

The boiling temperature was determined as the average boiling temperature obtained from Experiment 1 (196.80°C) and Experiment 3 (196.79°C).

Applicant's summary and conclusion

Conclusions:

The boiling temperature of Gyrane was determined at 197°C (470K) by using DSC. The atmospheric pressure was 1026 ± 1 hPa.

Executive summary:

The boiling temperature of Gyrane was determined at 197°C (470K) by using DSC. The atmospheric pressure was 1026 ± 1 hPa.