METHYL (1R,2R,4S)-2-[HEX-5-EN-1-YL(METHYL)CARBAMOYL]-4-({7-METHOXY-8-METHYL-2-[4-(PROPAN-2-YL)-1,3-THIAZOL-2-YL]QUINOLIN-4-YL}OXY)CYCLOPENTANECARBOXYLATE

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 March - 25 April 2016

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

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

methyl (1R,2R,4S)-2-[(hex-5-en-1-yl)(methyl)carbamoyl]-4-({7-methoxy-8-methyl-2-[4-(propan-2-yl)-1,3-thiazol-2-yl]quinolin-4-yl}oxy)cyclopentane-1-carboxylate

EC Number:

922-147-8

Cas Number:

1042695-87-3

Molecular formula:

C32H41N3O5S

IUPAC Name:

methyl (1R,2R,4S)-2-[(hex-5-en-1-yl)(methyl)carbamoyl]-4-({7-methoxy-8-methyl-2-[4-(propan-2-yl)-1,3-thiazol-2-yl]quinolin-4-yl}oxy)cyclopentane-1-carboxylate

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study reports): JNJ-39125593-AAA (T003019)
- Physical state: solid
- Appearance: white powder

Specific details on test material used for the study:

- Batch n°: M15FB2925
- Analytical purity: 99.5%
- Expiration date: 31 May 2017
- Storage condition: at room temperature protected from light

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

133.4 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

A charred residue remained after the preliminary and main test, indicating reaction and/or decomposition.

Decomp. temp.:

>= 325 °C

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 350°C. At 396°C the sample weight has decreased by 25%. After the experiment, a charred 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 was obtained with a heating rate of 20°C/min and showed an endothermic peak between 125°C and 175°C. The extrapolated onset temperature of the peak was 133.07°C. The effect was most likely obtained due to melting. An exothermic effect was observed between 325°C and 400°C. Reaction and/or decomposition is most likely the cause of this effect. After the experiment, a charred residue remained.

To investigate the melting peak between 125°C and 175°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 133.69°C. The melting temperature of T003019 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 133.4°C (407K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-39125593-AAA (T003019) was determined at 133.4°C (407K) by using DSC.