Sulfur fluorides, removal

Double asymmetric induction operates when the azomethine compound is derived from a chiral a-amino aldehyde and a chiral amine, e.g., the sulfin-imine 144 [70]. In this case, the R configuration at the sulfur of the chiral auxihary, N-tert-butanesulfinamide, matched with the S configuration of the starting a-amino aldehyde, allowing complete stereocontrol to be achieved in the preparation of the diamine derivatives 145 by the addition of trifluo-romethyl anion, which was formed from trifluoromethyltrimethylsilane in the presence of tetramethylammonium fluoride (Scheme 23). The substituents at both nitrogen atoms were easily removed by routine procedures see, for example, the preparation of the free diamine 146. On the other hand, a lower diastereoselectivity (dr 80 20) was observed in one reaction carried out on the imine derived from (it)-aldehyde and (it)-sulfinamide. 

The noteworthy advantages of the allyl ester are (a) it is readily introduced into amino acids (b) after isomerization (to 1-propenyl) by a palladium(O) catalyst it may be removed under weakly acidic or basic and neural conditions (32), even if sulfur-containing amino acids are present (34) (c) it shows orthogonal stability to the tert-butyloxycarbonyl and 9-fluorenylmethoxy-carbonyl groups (10) and (d) it is not affected by the hydrogen fluoride-pyridine complex (35). 

Metallic beryllium is produced by reduction of beryllium halide with sodium, potassium or magnesium. Commercially, it is obtained primarily from its ore, beryl. Beryllium oxide is separated from silica and alumina in ore by melting the ore, quenching the solid solution, and solubilizing in sulfuric acid at high temperatures and pressure. Silica and alumina are removed by pH adjustment. Beryllium is converted to its hydroxide. Alternatively, beryl is roasted with complex fluoride. The products are dissolved in water and then pH is adjusted to produce beryllium hydroxide. 

Sulfur analysis can normally be achieved successfully using modern elemental analyzers containing the usual tube packings but the addition of further chemical packings to specifically remove hydrogen fluoride can also remove sulfur dioxide and sulfur trioxide, so care has to be taken in their selection. Trifluoromethanesulfonate ion may be determined by ion chromatography under similar conditions to those for determining tetrafluoroborate. 

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