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Physical & Chemical properties

Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
7 January 2004 to 14 January 2004
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes
Type of method:
differential scanning calorimetry
Key result
Melting / freezing pt.:
> 158 - < 177 °C

Preliminary test

 

 Screening capillary

 Standard DSC (10 ºC/min)

 Tao

 179 ºC

 145 ºC

 Taend

 183 ºC

 191 ºC

 Teq

 125 ºC

 

 Tf

 201 ºC

 

Melting temperature by DSC test

 

 Test 1 (ºC)

 Test 2 (ºC)

 Mean (ºC)

 SD

 2SD

 Mean (ºK)

 Rounded Mean (ºK)

 Beginning of melt

 157.29

 159.46

 158.38

 1.1

 2.2

 431.53

 432

 Extrapolation onset

 167.69

 168.85

 168.27

 0.6

 1.2

 441.42

 441

 End of melt

 176.19

 177.44

 176.82

 0.6

 1.2

 449.97

 450

 

Based on the shape of the standard DSC curve and observations during the preliminary capillary test, the endothermic change in enthalpy observed at less than 155 °C was believed to be a change in crystalline structure. The test substance melted at 158-178 °C (432 - 450 °K). Estimated accuracy of the method was ± 2.2 °C.

Conclusions:
Under the conditions of the test, the melting point of the test substance was determined to be 158 - 177 ºC (432 - 450 ºK).
Executive summary:

In a GLP compliant melting point study conducted in line with EU Method A1, the boiling point of butanoic acid, 4-[[4-[7-chloro-6-(1,1-dimethylethyl)-3H-pyrazolo[1,5-b][1,2,4]triazol-2-yl]phenyl]amino-4-oxo, tetradecyl ester was determined using the differential scanning calorimetry method. The melting point of the substance was determined to be 158 - 177 ºC (432 - 450 ºK).

Description of key information

Key study:- Brandt (2004) 'Physico-chemical properties with respect to melting, boiling and solid flammability' conducted in line with EU Method A.1. The melting point of the test substance was determined to be 158-177 ºC (432-450 ºK).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
158 °C

Additional information

The key study (Brandt, 2004) was performed in compliance with GLP and to the EU Method A.1 with a sufficient level of detail to assess the quality of the presented data. The study was performed to a good standard in line with an accepted, standardised guideline and was assigned a reliability score of 1 using the principle for assessing data quality as set out in Klimisch et al. (1997). The melting point of the test substance was determined to be 158-177 ºC (432-450 ºK).