1-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2021-02-03 to 2021-04-13

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:

EU Method A.6 (Water Solubility)

Version / remarks:

March 04, 2016

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

July 27, 1995

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7840 (Water Solubility)

Version / remarks:

March 1998

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

column elution method

Test material

Test material information

Constituent 1

Reference substance name:

1-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Cas Number:

1903010-39-8

Molecular formula:

C25H23N7O5

IUPAC Name:

1-[2-[2-methoxy-4-(morpholin-4-yl)-5-nitroanilino]pyrimidin-4-yl]-3-phenyl-1H-pyrazole-4-carbaldehyde

Test material form:

solid: particulate/powder

Details on test material:

- Physical state: solid
- Appearance: orange powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Batch (Lot) Number: I20ED2016
- Purity/Composition: 101.5%
- Purity test date : 2020-07-27
- Expiry date: 2022-06-06 (retest date)
- Physical Description: Orange powder

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

Water solubility

Key result

Water solubility:

0.22 µg/L

Conc. based on:

test mat.

Remarks:

The water solubility of a test item is specified by the saturation mass concentration of the test item in water at a given temperature and is expressed in g/L or equivalent.

Temp.:

20 °C

pH:

> 7.5 - < 7.8

Remarks on result:

completely miscible

Details on results:

Preliminary Test:
The content of test item dissolved in the water sample was 2.89 µg/L.

The coefficient of variation (CV) (n = 5) was ≤ 30% at both flow rates. It demonstrated that the system was equilibrated at all flow rates.

The maximum difference (MD) on the mean values of the samples at both flow rates was also ≤30%. Based on this, the water solubility of the test item is given as the mean value of these measurements.

The turbidity of the eluates was < 0.2 NTU. According to this, no undissolved particles were detected in the eluates.

A small response at the retention time of the test item were detected in the chromatograms of the pretreated samples from the blank column. It was considered to derive from carry-over in the analytical system since similar responses were found in the analytical blanks. The maximum contribution to the samples was 12%. It was considered that it has no significant effect on the results of the test samples since last five fractions where concertation was constant within ± 30% were used to determine the solubility.

Any other information on results incl. tables

Main study - water solubility of the test item

Flow rate mL/h	Sample no.	Concentration analyzed					pH
		Individual [mg/L]	Mean^1	CV [%]	Mean^2 [mg/L]	MD [%]
24	1 2 3 4 5 6 7 8 9 10	0.00049 ^4 0.00026 4 0.00019 ^4 0.00020 ^4 0.00017 ^4 0.00018 0.00019 0.00021 0.00020 0.00019	0.00019	5.9	0.00022	26	7.8
12	1 2 3 4 5 6 7 8 9 10	0.0011 ^4 0.00042 ^4 0.00027 ^4 0.00025 ^4 0.00032 ^4 0.00027 0.00026 0.00025 0.00023 0.00025	0.00025	5.6			7.5

¹ Estimated value, calculated by extrapolation of the calibration curve
² Mean of the concentrations obtained at one flow rate
³ Mean of the concentrations obtained at both flow rates.
⁴ This value was not used for calculation of the mean because since cv for n=10 was >30%. Based on
guideline OEDC 105 at least five consecutive fractions where concertation is constant within ± 30% are
used to determine solubility.

Applicant's summary and conclusion

Conclusions:

The water solubility of the test item at 20°C was 0.00022 mg/L (0.22 µg/L).

The pH of the aqueous samples was 7.5 and 7.8.