1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22 July - 01 October 2015

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

Type of method:

thermal analysis

Specific details on test material used for the study:

- Batch n°: A14JB3422
- Analytical purity: 93.3%
- Expiration date: 30 September 2016
- Storage condition: at room temperature

Key result

Melting / freezing pt.:

ca. 120 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

>= 225 °C

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly starting at 275°C. At 467°C the sample weight has decreased by 25%. After the experiment, a black 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 showed an endothermic peak between 100°C and 150°C. The extrapolated onset temperature of the peak was 119.53°C. The effect was most likely obtained due to melting. A second endothermic peak was observed starting at 300°C due to reaction and/or decomposition of the test item. After the experiment, a 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 120.35°C. In the third experiment, the temperature program was stopped directly after the endothermic peak. The extrapolated onset temperature of the peak was 120.07°C. After the experiment, a white molten residue remained in the sample container. The result demonstrated that the endothermic effect was due to melting of the test item and that the exothermic effect was due to reaction and/or decomposition of the test item. The melting temperature of T001036 as the average melting temperature from Experiment 1 (119.53°C), Experiment 2 (120.35°C) and Experiment 3 (120.07°C) was 120°C (393K) by using DSC. Reaction and/or decompostion of T001036 was observed starting at 225°C (498K).

Conclusions:

The melting temperature of JNJ-119717-AAA (T001036) was determined at 120°C (393K) by using DSC.
Reaction and/or decomposition was observed starting at 225°C (498K).

Description of key information

A Klimisch 1 GLP study (WIL Research Europe, 2016) according to OECD Guideline 102, EU Method A.1 and EPA OPPTS 830.7200 reports a melting temperature of T001036 at 120°C by using DSC. Reaction and/or decomposition was observed starting at 225°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

120 °C