trans-(5RS,6SR)-6-amino-2,2-dimethyl-1,3-dioxepan-5-ol

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

19 Jan - 12 Feb 1993

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

67/548

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

other: capillary method, hot stages, differential scanning calorimetry, thermal analysis

Key result

Melting / freezing pt.:

81.7 °C

Remarks on result:

other: thermal analysis

Key result

Melting / freezing pt.:

> 69.4 - < 84.9 °C

Remarks on result:

other: DSC

Key result

Melting / freezing pt.:

> 65 - < 84 °C

Remarks on result:

other: hot stages

Key result

Melting / freezing pt.:

> 65 - < 84 °C

Remarks on result:

other: capillary method

Capillary method:
In the range from 65 °C to 70 °C, sintering and melting of parts of the test substance was observed. From 76 °C, the remaining part of the test substance began to melt and the end of the melting process was reached between 82 - 84 °C

Hot stages:
Partial melting of individual crystals was observed from 65 °C and a slight sublimation phenomenon from 72 °C on. The bulk of the sample showed a melting range between 80 °C and 84 °C.

DSC:
Temperature program: 1K/min in the range 25 °C to 100 °C.
The endotherm is divided into two regions, a minor peak between 63.9 °C to 69.4 °C and a subsequent main peak from 69.4 °C to 84.9 °C.

Thermal analysis:
Temperature program: 5K/min in the range approximately 30 °C to 120 °C.
First peak between approx. 40 °C to 66 °C, second peak 81.7 °C (extrapolated peakon set).

 

Validity criteria for the measurement of the meting point:

Target condition according to guideline:	Actual condition according to the study:	Validity criteria met:
The mean of at least two measurements which are in the range of the estimated accuracy is reported as the melting temperature. If the difference between the temperature at the beginning and at the final stage of melting is within the limits of the accuracy of the method, the temperature at the final stage of melting is taken as the melting temperature; otherwise the two temperatures are reported.	Different methods have been used for the determination of the melting point of the test substance. Since values were different, a melting range between 65 °C and 85 °C was specified.	yes
If the substance decomposes or sublimes before the melting temperature is reached, the temperature at which the effect is observed shall be reported.	The substance did not decompose before the melting temperature.	yes

Conclusions:

The melting range of the test substance is between 65 °C and 85 °C.

Executive summary:

The study was performed to assess the melting point. The study was conducted in accordance with EEC Method for "determination of the melting point", Directive 67/548/EEC, method A.1. Within the study the following methods were used: capillary method, hot stages, differential scanning calorimetry, thermal analysis. As a mean over all methods, the melting point of the test substance was determined as a range between 65 °C and 85 °C.

Description of key information

The study was performed to assess the melting point. The study was conducted in accordance with EEC Method for "determination of the melting point", Directive 67/548/EEC, method A.1. Within the study the following methods were used: capillary method, hot stages, differential scanning calorimetry, thermal analysis. As a mean over all methods, the melting point of the test substance was determined as a range between 65 °C and 85 °C.

Additional information

Melting range: 65 °C to 85 °C.