N-[3-(dimethylamino)propyl]dodecanamide N-oxide

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

10 Feb - 29 Apr 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2020

Report date:

2020

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

not specified

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

not specified

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

not specified

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

N-[3-(dimethylamino)propyl]dodecanamide N-oxide

EC Number:

263-218-7

EC Name:

N-[3-(dimethylamino)propyl]dodecanamide N-oxide

Cas Number:

61792-31-2

Molecular formula:

C17H36N2O2

IUPAC Name:

N-[3-(dimethylamino)propyl]dodecanamide N-oxide

Results and discussion

Melting / freezing point

Melting / freezing pt.:

>= 42.7 - <= 58.4 °C

Any other information on results incl. tables

Conclusion-

The melting temperature of N-[3-(dimethyloxidoamino)propyl]-dodecanamide (freeze dried) was determined by DSC. The melting range of the test item was 42.7 – 58.4°C (315.9 – 331.6K).

Details-

Preliminary Test:

Starting at 150°C, the weight of the sample decreased significantly. At 198°C, the sample weight had decreased by 25%. After the experiment, a brown molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

 

Main Study-

An endothermic effect was observed between 30°C and 70°C followed by the second endothermic effect between 90°C and 140°C and the third endothermic effect between 140°C and 198°C. The extrapolated onset temperature of the first effect could not be determined since the start of the effect was within 25°C from the start of the experiment. For this reason, the peak maximum of the first effect (i.e. 57.909°C) was not used in the calculation of the melting temperature. The first endothermic effect was most likely obtained due to melting of the test item or evaporation of volatile components. The origin of the second endothermic peak is unknown. The third endothermic effect was due to reaction and/or decomposition of the test item. After the experiment, a yellowish molten residue remained in the sample container (original colour: white). Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

To investigate the endothermic effect between 30°C and 70°C, a repeated heating cycle was applied in the Experiment 2. With the first heating, similar results were observed as in Experiment 1. The extrapolated onset temperature of the first effect could not be determined since the start of the effect was within 25°C from the start of the experiment. For this reason, the peak maximum of the first effect (i.e. 57.984°C) was not used in the calculation of the melting temperature. During cooling, two exothermic effects between 0°C and 85°C were found (results are archived in the raw data). These effects were obtained due to crystallization of the test item. With the second heating, an endothermic effect was observed between 0°C and 20°C with an extrapolated onset temperature of 13.940°C. Between 20°C and 100°C several endothermic and exothermic effects were observed. The origin of these effects is unknown. After the experiment, a white molten residue remained in the sample container.

In order to slow down evaporation of volatile components, a closed sample container was used in the Experiment 3. The first endothermic effect did not shift to higher temperatures, indicating melting of the test item. The extrapolated onset temperature of the first effect could not be determined since the start of the effect was within 25°C from the start of the experiment. For this reason, the peak maximum of the first effect (i.e. 57.960°C) was not used in the calculation of the melting temperature. The second endothermic effect which was observed in Experiment 1 between 90°C and 140°C, had shifted to a higher temperature, indicating evaporation of volatile components.

Exothermic decomposition effects were observed from 130°C. After the experiment, an orange molten residue remained in the sample container (original colour: white).

 

In order to determine the melting temperature, a lower start temperature was applied in the Experiment 4. The extrapolated onset temperature of the first part of the melting effect was 42.731°C. The peak maximum of the second part of the melting peak was 58.038°C. After the experiment, a white molten residue remained in the sample container.

Experiment 5 was performed as a duplicate of Experiment 4. Similar results as in Experiment 4 were obtained. The extrapolated onset temperature of the first part of the melting effect was 42.977°C. The peak maximum of the second part of the melting peak was 58.409°C. After the experiment, a white molten residue remained in the sample container. Since the melting effect has two peaks, a melting range will be given instead of a melting temperature. The melting range was determined as the lowest temperature and the highest temperature obtained in Experiment 4 and Experiment 5 (i.e. 42.731°C and 58.409°C).