โ Scribed by Prof. Dr. Hubert Schmidbaur; Dr. Georg Hasslberger; Ulrich Deschler; Dr. Ulrich Schubert; Dr. Charles kappenstein; Dr. Albin Frank
No coin nor oath required. For personal study only.
Hydroxy groups can, however, be readily protected by acylation and then, like other electronegative substituents, serve to direct the reaction of alkanes containing several tertiary C-H bonds.
Synthesis of cis-(3), X = O H : A mixture of cis-( 3), X = H (20 g, 0.145 mol) and (1 a) (20.3 g, 0.108 mol) (98 %, iodometric) in CHC13 (100ml) is heated under reflux for 7 h; after further addition of ( I a ) (20.3 g, 0.108 mol) and CHCl3 (30 ml), refluxing is continued for a further 16 h. The reaction mixture is then allowed to cool to room temperature, filtered, and the filter-cake washed with 350ml ether. The resulting organic phase is washed with 1 N NaOH and H20, and dried over Na2S04. The residue remaining after removal of solvent by distillation is found (gas-chromatographically) to contain 82 % cis-(3), X=OH. Distillation in a saber side-arm flask (b.p.
1 20-1 35 T / 2 0 torr) furnishes 15.6 g (69 %) of cis-( 3), X = OH, which is contaminated with 5% each of hydrocarbon and side-products.
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XAS at the nickel K-edge and UV-visible studies of rhombohedral nickel trifluoride indicate that the compound has a mixed valence composition Ni[NiF 6 ] and is isostructural with Pd[PdF 6 ]. XAS data are reported for NiF 2 , [NiF 6 ] 2ยฑ , [NiF 6 ] 3ยฑ , Pd[PdF 6 ], CoF 3 and RhF 3 in support of the N