The main fraction (6.65 g., theory 7.03 g.) was collected at 125-131°( 0.07 mm.). It was separated by further distillation into three fractions: (1) 2.6 g., b.p. 129-131°( 0.07 mm.); (2) 2.5 g., b.p. 132-135°( 0.1 mm.); and (3) residue, 0.6 g., which crystallized on standing.Fractions 1 and 2 (total 5.1 g.) are essentially pure diethyl-(4-ethoxy-2,3,5,6-tetramethylphenyl) phosphate ( ), »25d 1.4900, band at 7.9 µ. For analysis, fraction 2 was evaporatively distilled.
Formylcyclopentadienyl-(cyclopentadienyl) -iron, the first ferrocene derivative bearing an aldehyde function, has been synthesized by reaction of ferrocene with N-methylformanilide. A number of new diacylferrocenes have also been prepared by the Friedel-Crafts reaction. These new acyl derivatives, as well as the known acetylferrocene and diacetylferrocene, undergo many reactions characteristic of the carbonyl group.
A mechanism is proposed for the isomerization of olefins with compounds of rhodium, palladium, platinum, nickel, or iron as catalysts and with a variety of cocatalysts. A kinetically stable metal hydride with coordinated substrate olefin rearranges first to a metal alkyl, then to the metal hydride complex of the isomeric olefin.
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