Alkylation of 2-chlorophenol with isobutylene. The catalyst was prepared in the autoclave by heating 644 g. (5 moles) of 2-chlorophenol with 4.5 g. (V, formula wt.) of aluminum turnings. Alkylation with isobutylene was effected at 80-90°and the product worked up to give 550 g. (60%) of 2terí-butyl-6-chlorophenol (b.p. 123°at 30 mm.; n1 2D°1.5265).Anal. Caled, for Ci0Hi3C1O: Cl, 19.2. Found: Cl, 19.3. Proof of structure of 2-tert-butyl-6-chlorophenol. A portion of the product of the above experiment was chlorinated with sulfuryl chloride to yield 2,4-dichloro-6-ier<-butylphenol (for chlorination method see under structure proof of 2,6diisopropylphenol). The 2,4-dichloro-6-

No abstract

We wish to report the first alkyl derivatives of a metal carbonyl. Previous authors have reported the synthesis of cyclopentadienyl metal carbonyls1 and alkyl derivatives thereof2 3as well as acetylene and aliene corhplexes of metal carbonyls,8•4 ***but we know of no previous report of stable alkyl metal carbonyls.Manganese carbonyl dissolved in tetrahydrofuran was smoothly converted to a solution of NaMn(CO)6 when treated with an excess of 1% sodium amalgam or finely divided sodium in an inert atmosphere. This solution, maintained in the inert atmosphere, was decanted from excess sodium and treated with dimethyl sulfate or methyl iodide. Removal of solvent and recrystallization from petroleum ether followed by sublimation gave colorless crystals of methyl manganese pentacarbonyl, m.p. 94.5-95°( uncorr.).

No abstract

We wish to report the first alkyl derivatives of a metal carbonyl. Previous authors have reported the synthesis of cyclopentadienyl metal carbonyls1 and alkyl derivatives thereof2 3as well as acetylene and aliene corhplexes of metal carbonyls,8•4 ***but we know of no previous report of stable alkyl metal carbonyls.Manganese carbonyl dissolved in tetrahydrofuran was smoothly converted to a solution of NaMn(CO)6 when treated with an excess of 1% sodium amalgam or finely divided sodium in an inert atmosphere. This solution, maintained in the inert atmosphere, was decanted from excess sodium and treated with dimethyl sulfate or methyl iodide. Removal of solvent and recrystallization from petroleum ether followed by sublimation gave colorless crystals of methyl manganese pentacarbonyl, m.p. 94.5-95°( uncorr.).