4-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2021-01-12 to 2021-03-01

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2021

Report date:

2021

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Version / remarks:

August 1996

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point/Boiling Range)

Version / remarks:

July 27, 1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

March 04, 2016

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

4-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Cas Number:

2270944-70-0

Molecular formula:

C15H16ClN5O4

IUPAC Name:

4-chloro-N-[2-methoxy-4-(morpholin-4-yl)-5-nitrophenyl]pyrimidin-2-amine

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Batch (Lot) Number: I20CD1048
- Purity/Composition: 100%
- Purity test date : 2020-05-11
- Expiry date: 2022-03-22 (retest date)
- Physical Description: Light yellow to dark orange solid

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: At room temperature
- Stability and homogeneity of the test material in the vehicle/solvent under test conditions and during storage: not indicated
- Stability in the medium, i.e. sensitivity of the test material to hydrolysis and/or photolysis: not indicated
- Solubility and stability of the test material in the solvent/vehicle and the exposure medium: not indicated
- Reactivity of the test material with the incubation material used (e.g. plastic ware): not indicated

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
No treatment

OTHER SPECIFICS
- Purity/Composition correction factor: Yes, correction factor is 1.0

Results and discussion

Boiling point

Key result

Decomposition:

yes

Decomp. temp.:

225 °C

Remarks on result:

other: Boiling of the test item was not observed below the temperature at which reaction and/or decomposition started. Based on this, the test item has no boiling temperature

Any other information on results incl. tables

Preliminary Test
The TGA curve of the test item is shown in Figure 1. Starting at 200°C, the weight of the sample decreased significantly. At 374°C, the sample weight had decreased by 25%. After the experiment, a black charred residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item.

Main Study

In experiment 1, an endothermic effect directly followed by a strong exothermic was observed between 175°C and 225°C. The extrapolated onset temperature of the endo effect was 195.675°C. These effects were most likely obtained due to melting directly followed by reaction and/or decomposition of the test item.

After the experiment, a black charred residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, Experiment 2 was stopped directly after the melting effect. The extrapolated onset temperature was not determined since there is no entire peak showed. After the experiment, a black molten residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

In order to investigate the endothermic effect, a higher end temperature was used in the Experiment 3. The extrapolated onset temperature was 195.787°C. After the experiment, a black molten residue remained in the sample container (original colour: Light yellow to dark orange solid). The change of the colour indicated reaction and/or decomposition of the test item. Based on this visual observation, it was found that the test item had molten and the change of the colour demonstrated reaction and/or decomposition of the test item.

Reaction and/or decomposition of the test item were observed during DSC experiments during melting and directly after melting. Boiling of the test item was not observed below the reaction and/or decomposition T. Hence, the test item has no boiling point.

Applicant's summary and conclusion

Conclusions:

Boiling of the test item was not observed below the temperature of reaction and/or decomposition (>195.787°C). Based on this, the test item has no boiling temperature.