2-[[(2S)-2-(9H-fluoren-9-ylmethoxycarbonylamino)-3-(1H-imidazol-5-yl)propanoyl]amino]-2-methyl-propanoic acid Trifluoroacetic acid salt (1:1)

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15/11/2018-20/12/2018

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: Non-GLP study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2019

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: ASTM E 537-07

Deviations:

no

GLP compliance:

no

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

2-[(2S)-2-({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)-3-(1H-imidazol-5-yl)propanamido]-2-methylpropanoic acid; trifluoroacetic acid

EC Number:

815-122-7

Cas Number:

1446013-08-6

Molecular formula:

C27H27F3N4O7

IUPAC Name:

2-[(2S)-2-({[(9H-fluoren-9-yl)methoxy]carbonyl}amino)-3-(1H-imidazol-5-yl)propanamido]-2-methylpropanoic acid; trifluoroacetic acid

Test material form:

solid: particulate/powder

Details on test material:

Target Substance Molecular Formula: C27H27F3N4O7
Target Substance Molecular Weight: 576.51 g/mol
Batch Number: 160004
Physical form and colour: Solid, White powder
Storage: Store at 2÷8°C

Results and discussion

Boiling point

Remarks on result:

not determinable

Remarks:

It is not possible to define whether the peaks are imputable to a boiling point, and it is not known whether the boiling noted during the analysis with the melting point is attributable to a boiling or an effervescence of the sample.

Applicant's summary and conclusion

Conclusions:

Since it is not possible to define whether the peaks are imputable to a boiling point, and it is not known whether the boiling noted during the analysis with the melting point is attributable to a boiling or an effervescence of the sample, it is therefore considered that the point boiling point is not determinable.

Executive summary:

The aim of this test is the determination of the boiling point of N-[(9H-FLUOREN-9-YLMETHOXY)CARBONYL]-L-HISTIDYL-2-METHYLALANINE AND TRIFLUOROACETIC ACID (1:1); N.CAS

1446013 -08-6.

The test is performed in accordance to ASTM E 53707 (Differential scanning calorimetry method). It was not under GLP.

The sample is analyzed by means of the Dsc by executing this scan:

Weigh 5.425mg

1) Hold for 1.0 min at 0.00°C

2) Heat from 0.00°C to 250.00°C at 7.00°C/min

3) Cool from 250.00°C to 0.00°C at 7.00°C/min

4) Heat from 0.00°C to 250.00°C at 7.00°C/min

5) Cool from 250.00°C to 0.00°C at 7.00°C/min

6) Heat from 0.00°C to 20.00°C at 7.00°C/min

Subsequently a further scan is performed

Weighing 5,200mg

1) Hold for 1.0 min at 0.00°C

2) Heat from 0.00°C to 400.00°C at 5.00°C/min

3) Cool from 400.00°C to 0.00°C at 5.00°C/min

4) Heat from 0.00°C to 400.00°C at 5.00°C/min

5) Cool from 400.00°C to 0.00°C at 5.00°C/min

All the scans were carried out with a closed crucible, in an inert atmosphere of nitrogen.

The data obtained with the melting point apparatus:

• 167.1°C
• 164.7°C
• 162.4°C

From the 0-250 °C scan, the first temperature ramp (1), we note the presence of 3 peaks corresponding to

the temperature of:

• 184°C
• 191°C
• 202°C

From the second heating, no peak is known.

From the 0-40 °C scan, the first temperature ramp there are 3 peaks corresponding to the temperature:

• 186°C
• 191°C
• 198°C

From the second heating, no peak is known.

Since it is not possible to define whether the peaks are imputable to a boiling point, and it is not known whether the boiling noted during the analysis with the melting point is attributable to a boiling or an effervescence of the sample, it is therefore considered that the point boiling point is not determinable.