Reaction mass of 3-(difluoromethyl)-1-methyl-N-[(1RS,4SR,9RS)-1,2,3,4-tetrahydro-9-isopropyl-1,4-methanonaphthalen-5-yl]pyrazole-4-carboxamide and of 3-(difluoromethyl)-1-methyl-N-[(1RS,4SR,9SR)-1,2,3,4-tetrahydro-9-isopropyl-1,4-methanonaphthalen-5-yl]pyrazole-4-carboxamide; isopyrazam

Solubility in organic solvents / fat solubility

Link to relevant study record(s)

Reference

Endpoint:

solubility in organic solvents / fat solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

17 Jun 2008 to 28 Jun 2008

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: MT 157.3 “Flask Method” (Solubility above 10-2 g/L)

Version / remarks:

1995

GLP compliance:

yes (incl. QA statement)

Medium:

acetone

Solubility:

313.57 g/L

Temp.:

25 °C

Medium:

other: dichloromethane

Solubility:

330.16 g/L

Temp.:

25 °C

Medium:

ethyl acetate

Solubility:

178.85 g/L

Temp.:

25 °C

Key result

Medium:

other: hexane

Solubility:

1.17 g/L

Temp.:

25 °C

Medium:

methanol

Solubility:

119.13 g/L

Temp.:

25 °C

Medium:

n-octanol

Solubility:

44.13 g/L

Temp.:

25 °C

Medium:

toluene

Solubility:

77.13 g/L

Temp.:

25 °C

Test substance stable:

yes

Results

A saturated solution of the test item in each solvent (acetone, dichloromethane, ethyl acetate, hexane, methanol, octanol and toluene, respectively) was prepared by shaking a mixture of test item and solvent at 25 °C for 24 hours and 48 hours, respectively. The solutions were centrifuged, filtered and diluted.

The results of the individual measurements are given in Table 1 to Table 4 below.

To prove the suitability of the test system, seven solutions were prepared at a concentration near to the concentration of the sample solutions. These solutions were injected five times as SST. The relative standard deviations obtained were with less than 2.4 % below the limit of 5 %. The HPLC system was therefore considered to be suitable.

 

Table 1. Solubility in acetone and dichloromethane

Samp le No.	Weighed sample of the test item	Shaking time at 25 °C	Concen- tration analysed	Dilutionfactor before quanti- fication	Concen- tration calculated	Solubility calculated (rounded)
	[g]	[hours]	[mg/L]		[g/L]	[g/L]
Solvent: Acetone (5 mL)
1	2.01264	48	320.93	1000	320.93	313.57 SD = 13.39
			322.45		322.45
2	2.02813	48	321.17		321.17
			324.14		324.14
3	2.00274	24	295.30	1000	295.30
			297.45		297.45
4	2.00725	24	309.65		309.65
			313.67		313.67
Solvent: Dichloromethane (5 mL)
1	2.00720	48	327.87	1000	327.87	330.16 SD = 3.37
			325.15		325.15
2	2.00828	48	328.94		328.94
			332.97		332.97
3	2.03572	24	333.64	1000	333.64
			332.39		332.39
4	2.02828	24	359.53		359.53
			360.16		360.16

 

Table 2. Solubility in ethyl acetate and hexane

Samp le No.	Weighed sample of the test item	Shaking time at 25 °C	Concen- tration analysed	Dilutionfactor before quanti- fication	Concen- tration calculated	Solubility calculated (rounded)
	[g]	[hours]	[mg/L]		[g/L]	[g/L]
Solvent: Ethyl Acetate (5 mL)
1	2.01920	48	181.60	1000	181.60	178.85 SD = 8.14
			182.09		182.09
2	2.04607	48	185.28		185.28
			186.84		186.84
3	2.03918	24	168.39	1000	168.39
			168.91		168.91
4	2.00253	24	173.97		173.97
			176.31		176.31
Solvent: Hexane (5 mL)
1	0.06866	48	115.41	10	1.15	1.17 SD = 0.05
			115.89		1.16
2	0.07944	48	121.99		1.22
			123.04		1.23
3	0.06404	24	111.97	10	1.12
			111.61		1.12
4	0.06785	24	116.54		1.17
			117.45		1.17

 

Table 3. Solubility in methanol and octanol

Samp le No.	Weighed sample of the test item	Shaking time at 25 °C	Concen- tration analysed	Dilutionfactor before quanti- fication	Concen- tration calculated	Solubility calculated (rounded)
	[g]	[hours]	[mg/L]		[g/L]	[g/L]
Solvent: Methanol (5 mL)
1	2.05359	48	120.43	1000	120.43	119.13 SD = 2.44
			123.25		123.25
2	2.01326	48	118.71		118.71
			117.78		117.78
3	2.04955	24	232.38	500	116.19
			236.83		118.42
4	2.03238	24	233.00		116.50
			231.34		115.67
Solvent: Octanol (5 mL)
1	2.01731	48	44.29	1000	44.29	44.13 SD = 0.95
			45.13		45.13
2	2.01196	48	43.19		43.19
			42.76		42.76
3	2.01645	24	89.53	500	44.77
			89.36		44.68
4	2.03845	24	92.77		46.38
			93.77		46.88

 

Table 4. Solubility in toluene

Samp le No.	Weighed sample of the test item	Shaking time at 25 °C	Concen- tration analysed	Dilutionfactor before quanti- fication	Concen- tration calculated	Solubility calculated (rounded)
	[g]	[hours]	[mg/L]		[g/L]	[g/L]
Solvent: Toluene (5 mL)
1	2.04538	48	76.49	1000	76.49	77.13 SD = 1.14
			76.79		76.79
2	2.04677	48	76.31		76.31
			76.05		76.05
3	2.07045	24	157.03	500	78.52
			157.27		78.64
4	2.01389	24	156.61		78.30
			156.03		78.02

 

For the Tables above: the saturation mass concentration is calculated from the bold values given in the column “Concentration calculated”.

SD = standard deviation

Conclusions:

The solubility in seven organic solvents was found to range from 1.17 g/L in hexane to 330.16 g/L in dichloromethane.

Executive summary:

The solubility of test substance was determined in seven organic solvents according to CIPAC MT 157.3 (flask method) in compliance with GLP. The solubility in seven organic solvents was found to range from 1.17 g/L in hexane to 330.16 g/L in dichloromethane.

Description of key information

Solubility: The solubility was found to range from 1.17 g/L in hexane to 330.16 g/L in dichloromethane. CIPAC MT 157.3, Flask shake method, Weissenfeld 2008

Key value for chemical safety assessment

At the temperature of:

25 °C

Solubility in organic solvents at 20°C:

1.17 g/L