Fluka Chemie

For a review on silylating agents, see G. van Look, G. Simchen. and J. Heberle, Silylating Agents Fluka Chemie AG, 1995. 

Commercially available poly(a-D)galacturonic acid PGA) was purchased from Fluka Chemie. To obtain an aqueous solution of the polyacid, insoluble PGA was converted to its soluble sodium salt and then percolated through a cation-exchange resin in the H-form [3]. 

Initial efforts by workers at the Institute for Reference Materials and Measurement (IRMM), Geel, Belgium, to produce certified reference materials for GMOs have demonstrated that the provision of suitable reference materials is not easy and that together with the development of suitable analytical methods there are many challenges to be solved ahead. The first two examples produced jointly by the IRMM in Belgium and Fluka Chemie AG in Switzerland were based on Round-Up Ready Soya and BT 176 Maize. The reference materials are needed to validate EU and Swiss regulations which permit non-GMO products to be contaminated by up to 1 % GMO material and still be accepted. 

The submitters used PHB=Poly-(R)-3-hydroxybutyric acid obtained from Marlborough Biopolymers Ltd., Rudby Hall, Hutton Rudby, Yarm, Cleveland, England, PHB homopolymer, BX G04, technical grade powder, MBL 100/703. The checkers used PHB from Fluka Chemie AG, CH-8470 Buchs, Switzerland. The submitters report that the procedure works well on batch sizes of 200-250 g. 

The submitters report a yield of 45-48 g (74.5-79%) using PHB obtained from Marlborough Biopolymers. The checkers verified this result using PHB obtained from the submitters. The yield reported here represents the checker s results with PHB obtained from Fluka Chemie. 

DCM (anhydrous), DMSO (anhydrous), triethylamine (99 + %), sulfur trioxide-pyridine complex, DMA (anhydrous), potassium tert-butoxide (95%), DCE (anhydrous), 2-(4-methoxyphenyl)ethylamine (98 + %), sodium triacetoxy-borohydride (95%), A/A-diisopropylethylamine (99%), p-toluenesulfonyl chloride (99 + %), and trifluoroacetic acid (99 + %) were obtained from Aldrich Chemical Company, Inc. 4-Hydroxy-2-methoxybenzaldehyde (>98%) was obtained from Fluka Chemie, AG. 

G. van Look, Silylating Agents, Fluka Chemie, Buchs, 1988. 

Fluka Chemika, Chiral Compounds Chemistry, Fluka Chemie AG, Swit2erland, 1994. 

Compound 8 (40 mg) was dissolved in DMF (300 pL), FITC (40 mg) was added, and the mixture adjusted to pH 8.0 with NMM. After incubation for 15 h in the dark, the product was purified by chromatography (silica) on a Kieselgel 60 1.5 x 20-cm column (Fluka Chemie, Buchs, Switzerland) equilibrated in MeOH/CHCl3 (1 1). The excess FITC eluted in the flow-through fraction, and a second yellow fraction containing the expected product was eluted with MeOH/CHCl, (4 1). The solvent was removed by rotary evaporation, and the product was characterized by ESI-MS mlz. [M+H]+ calcd, 709.6 found, 709.4. Further purification was by semipreparative RP-HPLC on a Nucleosil-C8 column (10 x 250 mm) at a flow rate of 4mL min 1 using a 30-60% gradient (same components as above) over 30 min. 

N-Phenyl-P-naphthylamine (PBNA) - Fluka Chemie AG, Bucks, Switzerland... 

Alumina, aluminium oxide (Type 507C, neutral), can be obtained from Fluka Chemie AG, Industriestrasse 25, CH-9470, Buchs, Switzerland. 

S)-(-)-2-Methyl-1 -butanol (GC purity > 99.5% [a]p -6.6 0.3° (ethanol, c 10) was purchased from Fluka Chemie AG. Esterification with (R)-(+)-3.3,3-trifluoro-2-methoxy-2-phenylpropionic acid (Mosher s acid)2 and subsequent fH and 19F NMR analyses at 300 MHz of the resulting ester showed an enantiomeric purity of (S)-(-)-2-methyl-1-butanol > 99%. 

Materials. Trimethylamine N-oxide dihydrate (98%) from Aldrich and N-dimethyldodecylamine N-oxide (97%) from Fluka Chemie were used as received. N-dimethylhexylamine N-oxide and N-dimethyloctylamine N-oxide were prepared by reaction of the corresponding tertiary amine with hydrogen peroxide (12). Both samples were isolated as crystalline solids and were >99% pure, based on acid/base titrations and spectrometric methods. Both samples were very hygroscopic. Reagent grade NaBr, 0.1 N and 2.0 N HC1 were from J.T. Baker Chemical Co. and the all solutions were prepared using distilled and deionized water. The pH was monitored using an Orion Ross combination pH electrode and an Orion EA 940 meter. 

ABC buffer 50 mM aqueous ammonium bicarbonate (NH4HCO3) (BioChemika Ultra, >99.5%, Fluka Chemie GmbH store at room temperature). Check that pH is between 7.2 and 7.8. Store at room temperature. 

Iodoacetamide solution Dissolve 27.5 mg iodoacetamide (purum >98.0%, Fluka Chemie GmbH store at 4°C) in 100 jjlL water. Store at -20°C (see Note 4). 

Tert-butylbenzene (BDH Chemicals Ltd Poole, England) and dimethylmethylphosphonate (Fluka Chemie GmbH) were used as probe organic compounds in the breakthrough experiments. 

Palladium on barium sulfate was purchased from Fluka Chemie AG and pyridine (99.5%) was obtained from Chimie-Plus Laboratones (St.-Priest, France) and dried over calcium hydride before use. 

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