4H-Pyrido[1,2-a]pyrimidin-4-one, 3-(2-chloroethyl)-9-hydroxy-2-methyl-, hydrochloride (1:1)

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

23 September - 29 December 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

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-CHLOROETHYL)-9-HYDROXY-2-METHYL-4H-PYRIDO[1,2-A]PYRIMIDIN-4-ONE HYDROCHLORIDE (1:1)

EC Number:

617-648-0

Cas Number:

849727-62-4

Molecular formula:

C11H11ClN2O2.HCl

IUPAC Name:

3-(2-CHLOROETHYL)-9-HYDROXY-2-METHYL-4H-PYRIDO[1,2-A]PYRIMIDIN-4-ONE HYDROCHLORIDE (1:1)

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

- Name of test material (as cited in study report): T002006
- Substance type: almost white to ochre solid
- Physical state: solid
- Analytical purity: 97.5%
- Lot/batch No.: I15BB0722
- Expiration date of the lot/batch: 2017-02-21
- Storage condition of test material: At room temperature (15-25°C)

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

224.9 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

>= 224.9 °C

Remarks on result:

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

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 225°C. At 364°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: almost white to ochre). 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 showed an endothermic peak followed by several exothermic peaks between 175°C and 364°C. The extrapolated onset temperature of the endothermic peak was 225.32°C. The endothermic effect was most likely obtained due to melting. The exothermic effects were due to reaction and/or decomposition of the test item. After the experiment, a red/brown residue was observed on the lid of the sample container and a dark brown molten residue remained in the sample container. To investigate the endothermic peak, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 224.40°C. After the experiment, a light brown molten residue remained in the sample container. It demonstrated that melting and reaction and/or decomposition of the test item was the reason for the endothermic effect. The melting temperature of T002006 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 224.9°C (498.0K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-1692405-AAC (T002006) was determined at 224.9°C (498.0K) by using DSC.