Methyl DL-serinate hydrochloride

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

17 June 2014-07 September 2014

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP-compliant study in accordance with EC A.1, OECD 102 and EPA OPPTS 830.7200.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2014

Report date:

2014

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

(2008)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

(1995)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

(1998)

Deviations:

no

GLP compliance:

yes

Type of method:

thermal analysis

Remarks:

(differential scanning calorimetry)

Test material

Test material information

Constituent 1

Reference substance name:

Methyl DL-serinate hydrochloride

EC Number:

227-047-1

EC Name:

Methyl DL-serinate hydrochloride

Cas Number:

5619-04-5

Molecular formula:

C4H9NO3.ClH

IUPAC Name:

methyl 2-amino-3-hydroxypropanoate hydrochloride

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Details on test material:

- Name of test material (as cited in study report): DL-serine Methylester HCl
- Molecular formula: C4H9NO3.HCl
- Molecular weight: 155.58 g/mol
- Description: White crystalline powder
- Storage condition of test material: At room temperature in the dark
- Expiration date of the lot/batch: 14 September 2014

Results and discussion

Melting / freezing point

Melting / freezing pt.:

137 °C

Decomposition:

yes

Decomp. temp.:

> 150 °C

Remarks on result:

other: Melt. pt in K.: 410. Decomp. temp. in K: 423.

Any other information on results incl. tables

PRELIMINARY TEST WITH TGA

From 170°C upwards the weight of the sample decreased significantly. From 178°C upwards there was an abrupt decrease observed which indicates reaction and/or decomposition. After the experiment, a charred molten residue remained in the sample container and partially upon the lid.

 

DSC EXPERIMENTS

Experiment 1: An endothermic peak between 120°C and 160°C was observed, probably due to melting of the test substance. The extrapolated onset temperature of the peak was 136.97°C. After the experiment, a charred molten residue remained in the sample container. The change of the colour from white to black indicated reaction and/or decomposition.

 

Experiment 2: To investigate the peak between 120°C and 160°C a repeated heating cycle was applied.

-With the first heating the extrapolated onset temperature was 132.18°C.

-During cooling a small exothermic peak was observed between 120°C and 130°C due to crystallization of the test substance.

-With the second heating an extrapolated onset temperature of 131.75°C was obtained.

-After the experiment, a charred molten residue remained in the sample container.

 

Experiment 3: To determine if the endothermic effect was indeed due to melting of the test substance, heating was stopped at 150°C and the residue was visually inspected. Extrapolated onset temperature: 135.99°C. After the experiment, a white molten residue remained in the sample container from which it was concluded that the observed endothermic effect was indeed caused by melting of the substance.

 

Experiment 4: The temperature program was the same as in Experiment 1 and similar results were obtained. Extrapolated onset of the melting peak: 136.69°C. After the experiment, a charred (black) molten residue remained in the sample container.

 

The melting temperature of the substance was calculated from the values obtained in Experiment 1 (136.97°C) and Experiment 4 (136.69°C).

Applicant's summary and conclusion

Conclusions:

In a GLP-compliant study in accordance with EC A.1, OECD 102 and EPA OPPTS 830.7200 using differential scanning calorimetry, the melting temperature of the substance has been determined as 137°C. Decomposition of the substance started at 150°C.