Ethyl 4-oxopiperidine-1-carboxylate

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

04 September 2016 - 22 December 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7220 (Boiling Point / Boiling Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

Ethyl 4-oxopiperidine-1-carboxylate

EC Number:

249-984-5

EC Name:

Ethyl 4-oxopiperidine-1-carboxylate

Cas Number:

29976-53-2

Molecular formula:

C8H13NO3

IUPAC Name:

ethyl 4-oxopiperidine-1-carboxylate

Test material form:

liquid

Details on test material:

- Name of test material (as cited in study reports): JNJ-126971-AAA (T000509)
- Physical state: liquid
- Appearance: clear colourless to light yellow liquid

Specific details on test material used for the study:

- Batch n°: M15HB3826
- Expiration date: 13 January 2017
- Analytical purity: 98.5% (based on GC purity)
- Storage condition of test material: At room temperature

Results and discussion

Boiling point

Key result

Boiling pt.:

274.4 °C

Atm. press.:

ca. 1 022 hPa

Any other information on results incl. tables

During Experiment 2, an endothermic peak between 150°C and 300°C was observed. The effect was most likely obtained due to boiling of the test item. The extrapolated onset temperature of the peak was 274.174°C. After the experiment, a yellow spread out residue remained in the sample container.

During Experiment 3 a closed sample container was used to investigate the nature of the endothermic peak. During heating a small exothermic followed by an endothermic effect was observed between 150°C and 350°C. The extrapolated onset temperature of the endothermic peak was 321.428°C. After the experiment, the sample container was swollen. This was most likely due to the high pressure generated during the evaporation of the test item. The small exothermic signal might have been caused by a degradation reaction only occurring at elevated pressure. The fact that the endothermic signal was observed at higher temperatures when a closed sample container was used, indicated that the effect was most likely caused by boiling. After the experiment, a brown spread out residue remained in the sample container.

Experiment 4 was performed with a similar temperature program as Experiment 2. Similar results as with Experiment 2 were obtained. The extrapolated onset of the boiling peak was 274.228°C. After the experiment, a yellow spread out residue remained in the sample container.

To confirm that the endothermic peak derived from boiling (especially as a brown residue remained in the sample container after Experiment 3) a higher heating rate of 50°C/minute was applied in Experiment 5. The extrapolated onset temperature of the endothermic peak was 274.828°C. The similar value demonstrated that boiling of the test item was the reason for the endothermic effect.

The boiling temperature was determined as the average boiling temperature obtained from experiment 2 (274.174°C), experiment 4 (274.228°C) and experiment 5 (274.828°C).

Applicant's summary and conclusion

Conclusions:

The boiling temperature of JNJ-126971-AAA (T000509) was determined at 274.4°C (547.6K) by using DSC.