.beta.-D-Ribofuranoside, methyl 2,3-O-(1-methylethylidene)-, 5-(4-methylbenzenesulfonate)

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

February 22, 2005 to June 16, 2005

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: see 'Remark'

Remarks:

This study was conducted in compliance with the Swiss Ordinance relating to Good Laboratory Practice, adopted February 2nd, 2000 [RS 813.016.5. This Ordinance is based on the OECD Principles of Good Laboratory Practice, as revised in 1997 and adopted November 26th, 1997 by decision of the OECD Council [C(97)186lFinal].

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2005

Report date:

2005

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

Principles of method if other than guideline:

The above-mentioned guidelines contain several different methods for the determination of the melting point / melting range and the boiling point / boiling range. These are between others, thermal analysis using a calorimeter and visual tests (e.g. capillary method), where the melting resp. freezing temperatures as well as the boiling temperature are measured. In the present study the thermal analysis was applied.
A phase transformation, e.g. melting or evaporation, or a reaction, e.g. dissociation, usually is associated with a heat effect.
In the calorimeter, two identical aluminium sample containers, one filled with the test item and the other empty (used as the reference), were heated at a constant rate. During the experiment, the heat effect, i.e. the difference in heat flow between the sample container and the reference container, was registered.

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

[(3aS,4S,6S)-6-methoxy-2,2-dimethyl-tetrahydro-2H-furo[3,4-d][1,3]dioxol-4-yl]methyl 4-methylbenzene-1-sulfonate

EC Number:

609-920-2

Cas Number:

4137-56-8

Molecular formula:

C16H22O7S

IUPAC Name:

[(3aS,4S,6S)-6-methoxy-2,2-dimethyl-tetrahydro-2H-furo[3,4-d][1,3]dioxol-4-yl]methyl 4-methylbenzene-1-sulfonate

Details on test material:

Identity: Tosylfuranosid
Appearance: Solid / white
Storage: At room temperature at about 20°C
Expiration Date: July 31, 2005

Results and discussion

Boiling point

Decomposition:

yes

Decomp. temp.:

> 160 °C

Any other information on results incl. tables

RESULTS

The determination of the boiling point / boiling range of the test item was performed according to the EEC Directive 9 A.2 “Boiling temperature”, December 1992 and to the OECD Guideline No. 103: “Boiling Point”, adopted July 27, 1995.

Preliminary Test

The DSC-curve of the preliminary test (heating rate of 20 K/min from 25°C to 400°C) showed that there was no peak observed from which boiling of the sample could be deduced. After the experiment, the sample had lost about 69 % of its mass and the sample was black and carbonized.

Boiling Point

Using thermal analysis, no endothermic peaks were detected in the temperature range between 25°C and 400°C from which boiling could be deduced. During the preliminary test, an endothermic heat effect, the melting of Tosylfuranosid was observed at about 67.5°C. Starting at about 160°C an exothermic reaction was observed. The exothermic reaction was caused by the decomposition of the test item. After the experiment the test item was black and carbonized.

A second DSC run was performed to confirm the result found during the preliminary test.

In conclusion, the decomposition of Tosylfuranosid was observed before boiling occurred.

Applicant's summary and conclusion

Conclusions:

During this study the boiling point of Tosylfuranosid was determined.
No boiling point could be determined as decomposition of Tosylfuranosid was observed before boiling occurred.

Executive summary:

Using thermal analysis, no endothermic peaks were detected in the temperature range between 25°C and 400°C from which boiling could be deduced. During the preliminary test, an endothermic heat effect, the melting of Tosylfuranosid was observed at about 67.5°C. Starting at about 160°C an exothermic reaction was observed. The exothermic reaction was caused by the decomposition of the test item. After the experiment the test item was black and carbonized.

A second DSC run was performed to confirm the result found during the preliminary test.

In conclusion, the decomposition of Tosylfuranosid was observed before boiling occurred.