Tricyclo[3.3.1.13,7]decane-1-acetic acid, .alpha.-[[(1,1-dimethylethoxy)carbonyl]amino]-3-hydroxy-, (.alpha.S)-

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

31 December 2004 to 23 May 2005

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study was conducted in 2005 according to EU and OECD Method and in accordance with GLP. The study material is well characterized

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2005

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling point/boiling range)

Deviations:

no

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

(2S)-2-{[(tert-butoxy)carbonyl]amino}-2-(3-hydroxyadamantan-1-yl)acetic acid

EC Number:

700-361-0

Cas Number:

361442-00-4

Molecular formula:

C17H27NO5

IUPAC Name:

(2S)-2-{[(tert-butoxy)carbonyl]amino}-2-(3-hydroxyadamantan-1-yl)acetic acid

Constituent 2

Reference substance name:

1-Hydroxyadamantanyl-3-(S)-Boc-glycine

IUPAC Name:

1-Hydroxyadamantanyl-3-(S)-Boc-glycine

Details on test material:

31 December 2004 to 23 May 2005

Results and discussion

Boiling point

Boiling pt.:

ca. 304.6 °C

Decomposition:

yes

Decomp. temp.:

ca. 380 °C

Any other information on results incl. tables

Test 1 A melting endotherm was observed with a peak temperature of 180.0°C. A second endotherm was observed, due to the boiling point, with a peak temperature of 303.3°C. An unsteady baseline was subsequently observed, starting at ca. 380°C, indicative of decomposition of residue. Test 2 A melting endotherm was observed with a peak temperature of 180.3°C. A second endotherm was observed, due to the boiling point, with a peak temperature of 305.8°C.

Applicant's summary and conclusion

Conclusions:

The thermal behaviour of BMS 528233-01 was assessed by Differential Scanning Calorimetry. A melting endotherm was observed with a peak temperature of 180.2°C. A second endotherm was observed, due to the boiling point, with a peak temperature of 304.6°C. An unsteady baseline was also observed, starting at ca. 380°C, indicative of decomposition of residue.

Executive summary:

A melting endotherm was observed with a peak at 180.2°C, followed by a probable boiling endotherm with a peak temperature of 304.6°C. The melting point is defined as the temperature at which the phase transition from solid to liquid state takes place. Similarly, the boiling point is defined as the temperature at which the saturated vapour pressure of a liquid is the same as the standard (atmospheric) pressure. Both the melting and boiling point of the test substance were determined by differential scanning calorimetry (DSC). This is a technique in which a sample and a thermally inert reference material are subjected to a programmed temperature increase that is linearly ramped with time. The sample or reference is heated to maintain zero temperature difference, and the energy is plotted as a function of the programmed temperature. This provides a direct calorimetric measure of the energy of the reaction or transition. For example, if substance and empty reference pans are heated over the test substance's solid to liquid-phase transition temperature, the energy required to melt the test substance can be determined along with the actual melting temperature. The boiling or decomposition parameters can similarly be determined.