(±)-7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]thiazepin-11-yl)amino]heptanoic acid S,S-dioxide

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

August to november 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Justification for type of information:

The determination was carried out by differential scanning calorimetry, using a procedure designed to be compatible with Method A.1 Melting/Freezing Temperature of Commission Regulation (EC) No440/2008 of 30 May 2008 and Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July
1995

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

(±)-7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]thiazepin-11-yl)amino]heptanoic acid S,S-dioxide

EC Number:

276-851-9

EC Name:

(±)-7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]thiazepin-11-yl)amino]heptanoic acid S,S-dioxide

Cas Number:

72797-41-2

Molecular formula:

C21H25ClN2O4S

IUPAC Name:

(±)-7-[(3-chloro-6,11-dihydro-6-methyldibenzo[c,f][1,2]thiazepin-11-yl)amino]heptanoic acid S,S-dioxide

Test material form:

solid: crystalline

Details on test material:

White powder

Specific details on test material used for the study:

Batch18114773 - purity > 99.5%
The temperature accuracy of the DSC was checked prior to testing with indium and zinc. These were within defined tolerances and the DSC was therefore considered acceptable for use.
Aliquots of test item (see following table) were placed in pierced crucibles and were subjected to a thermal program from 80 to 180 °C at 1 °C/min.
The appearance of the samples (residue) was recorded after the test.

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

> 145.9 - < 146.9 °C

Any other information on results incl. tables

Thermal event	Interpretation	Temperature (°C)
		Determination 1	Determination 2
Endotherm 1 extrapolated onset temperature	Extrapoled onset of possible polymeric changes	137.6	137.68
Endotherm 1 extrapolated onset temperature	Extrapoled onset of melting	146.42	146.44

On thermal analysis, two distinct, consistent endothermic events were observed, possibly indicative of a polymorphic nature to the test item. A visual assessment of the melting characteristics of the test item, performed using a metal block apparatus, confirmed a broad melting temperature range for the test item starting at 143 °C. Additional cyclic differential scanning calorimetry, utilizing a temperature program of 125 to 142 °C at 1 °C/min, reduce temperature to 120 °C with a second heating to 142 °C at 1 °C/min was carried out. This cyclic determination showed only a single peak, allowing the first endotherm at approximately 137 °C to be excluded as an endotherm associated with melting.

Applicant's summary and conclusion

Conclusions:

The melting point of the test item has been determined to be 146.4 ± 0.5°C (419.6 ± 0.5 K).

Executive summary:

The melting point of the test item has been determined to be 146.4 ± 0.5°C (419.6 ± 0.5 K). Testing was performed by a differential scanning calorimetry procedure designed to be compatible with Method A.1 Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.