## Assessment of Purity (Interim Results)

Report for

Project Number: 13714

Prepared by

Alison M. McGuire BSc CSci CChem FRSC

Compliance Services International ‐ Europe

Pentlands Science Park, Penicuik

Nr. Edinburgh, EH26 0PZ
www.ComplianceServices.comPage 3 EXECUTIVE SUMMARY 1

The objective of this work was to evaluate the purity of two batches of (Batches 12166 and 12342).

The purity has been determined by subtracting the percentage of impurities detected due to the unavailability of a reference standard for

The following techniques have been used to assess th e puri t y of

 Liquid Chromatography with Mass Spectroscopy (LC

‐ MS)

 Gas Chromatography with Mass Spectroscopy (GC

‐ MS)

Supporting Data

 Proton and Boron Nuclear Magnetic Resonance ( 1 H and 11 B NMR) (Batch 13337)

 X

‐ Ray Diffraction (XRD) (Batch 13337)

Based on the manufacturing process it was considered that the following impurities could theoretically be present in






Scans were performed using the techniques identified above and no other substances were found to be presen t. was found to be present at ca. , was found to be present at ca. , and was not found (<0.1%). These figures are suggestive of a purity of Work is ongoing to confirm these interim results.

Chemical Characteristics 1.1

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular W e ight: 469
Physical State: White crystalline powder

Arrival Date: 11 Jan 2012 (Batch 12166)

19 March 2013 (Batch 12342)

Expiry Date: 10 April 2014 1 (Both batches)

Storage Conditions: Room temperature (15

‐ 30°C)

1 Assigned by the testing laboratory.Page 4 Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular Weight: 138.120697
Physical State: colourless to white crystals

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular W e ight: 185.349503
Physical State: Colourless to yellow liquid

Name:

Chemical Structure:

CAS Number:

Chemical Formula:

Molecular W e ight: 61.833
Physical State: White crystalline solidPage 5 Determination 1.2 (Smithers Viscient Letter Report, SABoTBA Ref.3200166, 12 December 2013, Appendix I)

LC

‐ MS analysis found ca. w/w

.

e

GC

‐ MS analysis found ca. w/w

.

Determination 1.3 (University of Sheffield 1 H and 11 B NMR Spectra, Appendix II; Ceram X

‐ Ray Diffraction Quantitative Phase Analysis Report, Appendix III)

From the results of the NMR analysis it can be concluded that there is no present at levels

≥ 0.1%.

A sample of was fortified at this level and measured using both proton and NMR to confirm that the instrum ent could accurately measure at this concentration. A peak was observed when fortified (5.6 ppm 1 H; 24.962 ppm 11 B), confirming that the method is sufficiently

sensitive for

. No peak was detected in the sample unfortified with

, thus demonstrating that there is no present in the sample at

.

X

‐ ray diffraction did not determine the presence of any at levels (the in st rument
limit of detection).

Conclusion 2

Based upon interim data the purity of SABoTBA can be described as shown below: ‐

Chemical Substance Percentage w/wPage 6 Appe ndix I Let ter Report from Smithers ViscientPage 8 Appe ndix II Universi ty of Sheffield 1 H and 11 B NMR Spectra

### -0 .5 ppm S a m p l e r ef

. -13337- II i n CDC l3

Current Data Parameters NAME Nov21 EXPNO 501 PROCNO 1

F2 - Acquisition Parameters Date_ 20131121 Time 9.20 INSTRUM drx500 PROBHD 5 mm BBI 1H-BB PULPROG zg30 TD 65536 SOLVENT CDCl3 NS 32 DS 4 SWH 5995.204 Hz FIDRES 0.091480 Hz AQ 5.4657526 sec RG 128
DW 83.400 usec DE 6.00 usec TE 298.0 K D1 0.10000000 sec TD0 1

======== CHANNEL f1 ======== NUC1 1H P1 7.68 usec PL1 -3.00 dB SFO1 500.1323530 MHz

F2 - Processing parameters SI 32768 SF 500.1300177 MHz
WDW no SSB 0
LB 0.00 Hz GB 0 PC 1.00

F2 - Spectrum reference SR 17.74 Hz

F2 - Digital resolution: Hz per point HZpPT 0.182959 Hz

### -0 .5

10 .5 10 .0 9 .5 9 .0 8 .5 8 .0 7 .5 7 .0 6 .5 6 .0 5 .5 5 .0 4 .5 4 .0 3 .5 3 .0 2 .5 2 .0 1 .5 1 .0 0 .5 0 .0 ppm S a m p l e r ef

. dop e d w i t h at 0

. 1 % i n CDC l 3 + a drop o f D M SO

Current Data Parameters NAME Nov29 EXPNO 524 PROCNO 1

F2 - Acquisition Parameters Date_ 20131129 Time 16.46 INSTRUM drx500 PROBHD 5 mm BBI 1H-BB PULPROG zg30 TD 65536 SOLVENT CDCl3 NS 32 DS 4 SWH 5995.204 Hz FIDRES 0.091480 Hz AQ 5.4657526 sec RG 128
DW 83.400 usec DE 6.00 usec TE 298.0 K D1 0.10000000 sec TD0 1

======== CHANNEL f1 ======== NUC1 1H P1 7.68 usec PL1 -3.00 dB SFO1 500.1323530 MHz

F2 - Processing parameters SI 32768 SF 500.1300177 MHz
WDW no SSB 0
LB 0.00 Hz GB 0 PC 1.00

F2 - Spectrum reference SR 17.72 Hz

F2 - Digital resolution: Hz per point HZpPT 0.182959 Hz 

### Proton Nuclear Magnetic Resonance (1H NMR) (Batch 13337) Fortified with 0.1%

### Sample ref. -13337-II in CDCl3

Backwards linear prediction parameters: NCOEF = 2048 TDOFF = 32

-80 -70 ppm5 Current Data Parameters NAME Nov21 EXPNO 700 PROCNO 1

F2 - Acquisition Parameters Date_ 20131121 Time 9.15 INSTRUM drx500 PROBHD 5 mm BBI 1H-BB PULPROG zg TD 65402 SOLVENT CDCl3 NS 129 DS 0 SWH 32051.281 Hz FIDRES 0.490066 Hz AQ 1.0203212 sec RG 256
DW 15.600 usec DE 6.00 usec
TE 298.0 K D1 0.10000000 sec TD0 1

======== CHANNEL f1 ======== NUC1 11B P1 25.00 usec PL1 -3.00 dB SFO1 160.4620000 MHz

F2 - Processing parameters SI 32768 SF 160.4615790 MHz WDW EM SSB 0 LB 5.00 Hz GB 0 PC 1.40

F2 - Spectrum reference SR -421.00 Hz

F2 - Digital resolution: Hz per point HZpPT 0.978127 Hz 

### Boron Nuclear Magnetic Resonance (11B NMR) (Batch 13337)

### Sample ref. doped with at 0.1 % in CDCl3 + Drop of DMSO 4210832n Backwards linear prediction parameters: NCOEF = 2048 TDOFF = 32

-65 -60 -55 -50 5 ppm8471962 Current Data Parameters NAME Nov29 EXPNO 725 PROCNO 1

F2 - Acquisition Parameters Date_ 20131129 Time 16.04 INSTRUM drx500 PROBHD 5 mm BBI 1H-BB PULPROG zg TD 65402 SOLVENT CDCl3 NS 760 DS 0 SWH 32051.281 Hz FIDRES 0.490066 Hz AQ 1.0203212 sec RG 256
DW 15.600 usec DE 6.00 usec
TE 298.0 K D1 0.10000000 sec TD0 1

======== CHANNEL f1 ======== NUC1 11B P1 25.00 usec PL1 -3.00 dB SFO1 160.4620000 MHz

F2 - Processing parameters SI 32768 SF 160.4615790 MHz WDW EM SSB 0 LB 5.00 Hz GB 0 PC 1.40

F2 - Spectrum reference SR -421.00 Hz

F2 - Digital resolution: Hz per point HZpPT 0.978127 Hz 

### Boron Nuclear Magnetic Resonance (11B NMR) (Batch 13337) Fortified with 0.1%Page 13 Appe ndix III Ceram X

‐ Ray Diffraction Quantitative Phase Analysis Report

### MICROSTRUCTURE ANALYSIS REPORT

Client: Ceram Reference: (135995)-25352

For the Attention of:

Date Logged:

Date of Tests: 21-Nov-2013 22-Nov-2013 to 20-Nov-2013

Report Date: 22-Nov-2013

7679-ANJ Purchase Order No.:

Ceram UK Work Location: Test Method: Description: Examination by X-Ray Diffraction

Methods M7, M9 and M30

Please find attached the results for the sample(s) recently submitted for analysis.
Opinions and interpretations expressed herein are outside the scope of UKAS Accreditation.

2

Author Dr Giles Blundred

Page 1 of 2 pages

is taken for the accuracy of the sampling unless this is done under our own supervision. This report shall not be reproduced in part without the written This report is issued in accordance with the Conditions of Business of Ceram Research Limited and relates only to the sample(s) tested. No responsibility

approval of Ceram Research Limited, nor used in any way as to lead to misrepresentation of the results or their implications.

Ceram is the trading name of Ceram Research Limited. Registered in England No. 1960455 Registered Office as above.

0013Ceram Reference: (135995)-25352 Customer Reference: – 13337 - II Description:

Page 2 of 2 pages Quantita tiv e Examination by X-Ray Diffraction

An organic colour developer sample was submitted for Quantit ative Phase Analysis by X-Ray Diffraction in order to assess the presence of The sample was evaluated in accordance with UKAS

accre d ited in-house methods, M7, M9 and M30. Due to the unknown structure of the target compound a spinel standard was added to the sample to act as an internal standard.

Your Reference – 13337 - II

Phase Content

Not detected

End of Test Repor t