3-(2-hydroxyethyl)-1H,3H-quinazoline-2,4-dione

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-02-03 to 2017-05-19

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

3-(2-hydroxyethyl)-1H,3H-quinazoline-2,4-dione

EC Number:

214-897-3

EC Name:

3-(2-hydroxyethyl)-1H,3H-quinazoline-2,4-dione

Cas Number:

1207-75-6

Molecular formula:

C10H10N2O3

IUPAC Name:

3-(2-hydroxyethyl)-1,2,3,4-tetrahydroquinazoline-2,4-dione

Test material form:

solid

Specific details on test material used for the study:

- Batch n°: I16JB3859
- Analytical purity: 99.4%
- Expiration date: 2018-10-15
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

254.5 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A black molten residue remained after the preliminary test and a white molten residue remained after the main test, indicating reaction and/or decomposition.

Decomp. temp.:

> 275 °C

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 325°C. At 492°C the sample weight has decreased by 25%. After the experiment, a black 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 tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min was obtained and showed an endothermic peak between 250°C and 275°C. The extrapolated onset temperature of the peak was 254.61°C. The effect was most likely obtained due to melting. An exothermic deviation from the baseline started from 350°C. The effect was most likely due to reaction and/or decomposition of the test item. After the experiment, a white molten residue remained in the sample container.

During the preliminary test weight loss was observed from 275°C. To investigate this weight loss a lower heating rate of 5°C/minute was applied in the Experiment 2.

The extrapolated onset temperature of the melting peak was 254.36°C. The similar value obtained demonstrated that melting of the test item was the reason for the endothermic effect. Since a lower heating rate was applied, the extrapolated onset was not used for calculating the melting temperature. A small endothermic peak followed by an exothermic peak was observed from 275°C.

Experiment 3 was performed to determine the duplicate melting temperature of the test item. The experiment was stopped after the melting peak at 275°C. The extrapolated onset of the melting peak was 254.39°C.

The melting temperature of T001200 was determined as the average melting temperature obtained from Experiment 1 and Experiment 3 equals 254.5°C (527.7K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-369215-AAA (T001200) was determined at 254.5°C (527.7 K) by using DSC.