2-ethoxy-5-(4-methyl-1-piperazinylsulfonyl)benzoic acid

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

16 August and 28 September 1995

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted according to OECD and EUand in accordance with GLP. Study material is well characterized.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

1997

Report date:

1997

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

Commission Directive 92/69/EEC, A2 (differential scanning calorimetry method).

Deviations:

no

Principles of method if other than guideline:

The technique of Differential Scanning Calorimetry was employed, using the methods described in the ASTME standards: 537-76 (the standard method for assessing the thermal stability of chemicals by methods of differential thermal analysis), 473-85 (Standard definition of terms relating to thermal analysis) and 472-86 (Standard practice for reporting thermoanalytical data) and in accordance with OECD Guideline 113.

Test substance was weighed into five aluminium crucibles (ca 9 mg in each) and aluminium oxide (ca
9 mg) weighed into another crucible. A perforated lid was cold welded onto each crucible.

Preliminary tests were performed to determine the melting/decomposition temperature range and the boiling/decomposition temperature range. The definitive test was performed in duplicate, using a fresh sample in each case.

The crucible containing the aluminium oxide was used as a reference for all the tests. A nitrogen purge of 30 ml/minute was employed in each test.
The calorimeter was connected to a printer and traces of each test obtained. The test substances crucibles were inspected after each test.

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Test material form:

other: White to off white crystalline solid

Details on test material:

Identity: UK-143,108
Chemical name: 2-Ethoxy-5-(4-methyl-1- piperazinesulphonyl)benzoic acid
Expiry: 19 November 1995
Purity: 99.6% (excluding organic solvents)
Appearance: White to off white crystalline solid
Storage conditions: Dark at room temperature
Date received: 19 May 1995

Results and discussion

Boiling point

Key result

Boiling pt.:

> 275 - < 310 °C

Atm. press.:

other: atmosphere

Decomposition:

yes

Remarks:

at melting

Decomp. temp.:

> 189 - < 196 °C

Any other information on results incl. tables

Two endotherms were recorded from test substance scans The first endotherm between 189°C and 207°C (test 2 and 3) agreed with the melting point determination (test Al). A second DSC on the same sample showed no endotherm indicating decomposition on melting. The second endotherm between 275°C and 310°C indicated decomposition at the boiling temperature as inspection of the test crucible after the test showed that a red/brown solid had been produced

Applicant's summary and conclusion

Conclusions:

UK-143,108 underwent decomposition on melting between 189°C and 196°C and on boiling between 275°C and 310°C.