3-(2-chloroethyl)(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:

08 September - 03 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)(1H,3H)quinazoline-2,4-dione

EC Number:

225-795-3

EC Name:

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

Cas Number:

5081-87-8

Molecular formula:

C10H9ClN2O2

IUPAC Name:

3-(2-CHLOROETHYL)QUINAZOLINE-2,4(1H,3H)-DIONE

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study report): JNJ-232726-AAA (T001201)
- Physical state: solid
- Appearance: off-white powder
- Analytical purity: >99.16%
- Batch n°: I15CB1185
- Expiration date: 15 March 2017
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

ca. 195.3 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 275 °C

Remarks on result:

other: A black molten residue remained after the preliminary test and a red/purple/brown molten residue was obtained 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 from 275°C. At 475°C the sample weight has decreased by 25%. After the experiment, a black molten residue remained in the sample container (original colour: off-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 showed two endothermic peaks between 150°C and 225°C. The extrapolated onset temperatures of the peak were 183.60°C and 195.21°C. The effects were most likely obtained due to melting of the test item. An exothermic peak started at 275°C due to reaction and/or decomposition of the test item. After the experiment, a red/purple molten residue remained. To investigate the melting peak between 150°C and 225°C, a repeated heating cycle was applied. The extrapolated onset temperatures of the melting peak were 183.63°C and 195.37°C. A lower heating rate of 5°C/min was applied in a third experiment. The extrapolated onset temperatures of the melting peaks were 178.75°C and 194.31°C. After the experiment a colourless molten residue remained. The first peak shifted slightly to a lower temperature. After visual observations in combination with the results from the preliminary test, it could be concluded that the peak was not caused by reaction and/or decomposition of the test item.

Based on the information provided by the sponsor, the substance has a melting temperature of 190°C. Therefore the main peak at 195°C is chosen as the melting point, while the small peak at 184°C is attributed to recrystallization. The melting temperatur is determined as the average melting point of Experiment 1 (195.21°C) and Experiment 2 (195.37°C), which equals 195.3°C (468K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-232726-AAA (T001201) was determined at 195.3°C (468K) by using DSC.