3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

01 February 2017 - 13 July 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

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)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

EC Number:

255-207-0

EC Name:

3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Cas Number:

41078-70-0

Molecular formula:

C11H11ClN2O

IUPAC Name:

3-(2-chloroethyl)-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study report): JNJ-559728-AAA (T001250)
- Physical state: solid (powder)
- Appearance: White powder

Specific details on test material used for the study:

- Batch n°: I16DB2043
- Analytical purity: 99% (based on base titration assay)
- Expiration date: 25 April 2020
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

143.6 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 275 °C

Remarks on result:

other: A brown to black molten residue remained after the preliminary and 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 280°C. At 314°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 125°C and 175°C. The extrapolated onset temperature of the peak was 143.6°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 275°C due to reaction and/or decomposition of the test item. After the experiment, a black molten residue remained. To investigate the melting peak between 143.6°C and 143.5°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 143.5°C. The melting temperature of T001250 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 143.6°C (416.7K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-559728-AAA (T001250) was determined at 143.6°C (416.7K) by using DSC.