cis-2-(bromomethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane-4-ylmethyl benzoate

Melting point / freezing point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

supporting study

Reliability:

4 (not assignable)

Rationale for reliability incl. deficiencies:

other: Documentation insufficient for assessment. No information on purity of the substance.

Guideline:

other: no data

GLP compliance:

not specified

Type of method:

thermal analysis

Melting / freezing pt.:

115 °C

Conclusions:

The melting point of T001095 is approximately 115 °C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 November 2016 - 06 February 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

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

Specific details on test material used for the study:

- Batch n°: I15DB1648
- Expiration date: 19 April 2020
- Purity: 96.70% (based on chromatographic purity)
- Storage condition of test material: at room temperature

Key result

Melting / freezing pt.:

116.8 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Remarks:

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

Decomp. temp.:

> 300 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 300°C. At 315°C the sample weight has decreased by 25%. After the experiment, a dark brown molten 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 with a heating rate of 20°C/min was obtained and showed an endothermic peak between 100°C and 150°C. The extrapolated onset temperature of the peak was 116.515°C. The effect was most likely obtained due to melting. After the experiment, a dark brown molten residue remained. To investigate the melting peak between 100°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 117.047°C. The melting temperature of T001095 was determined as the average melting temperature obtained from Experiment 1 and Experiment 2 and equals 116.8°C (389.9K).

Conclusions:

The melting temperature of JNJ-16479671-AAA (T001095) was determined at 116.8°C (389.9K) by using DSC.

Description of key information

In a GLP study according to OECD guideline 102, EU method A.1 and EPA OPPTS 830.7200 (Klimisch 1, Ciric, 2017) the melting point of T001095 was determined to be 116.8°C (389.9K).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

116.8 °C

Additional information

A supporting study (Janssen Pharmaceutica Process Safety Center, 1997) with insufficient documentation, and therefore assigned as Klimisch 4 study, concluded that the melting temperature of T001095 is about 115°C, which is in line with the result of the key study by Ciric (2017).