Ann Keep

Sequential one-pot bimetallic Ir(III)/Pd(0) catalysed mono-/bis-alkylation and spirocyclisation processes of 1,3-dimethylbarbituric acid and allenes

Microwave assisted indirect functionalization of alcohols with 1,3-dimethylbarbituric acid followed by spirocyclisation employing a sequential one-pot Ir(III)/Pd(0) catalysed process, involving the formation of three new C-C bonds, one spirocyclic ring and one di- or tri-substituted exocyclic alkene, is described.

Isoindolinones via a room temperature palladium nanoparticle-catalysed 3-component cyclative carbonylation–amination cascade

Abstract A room temperature 3-component cascade process involving nucleophilic substitution/carbonylation/amination, catalysed by palladium nanoparticles generated in situ from palladacycle 5 , affords isoindolinones in good yields. The conversions correlate with the p K a values of the amines.

Ru3(CO)9BH5 and [Ru3(CO)9BH4]- as precursors to higher nuclearity homo- and heterometallic clusters : molecular structure of a second isomer of HRu6(CO)17B

Abstract The cluster Ru 3 (CO) 9 BH 5 , which ontains four bridging (RuHRu or RuHB) hydrogen atoms, spontaneously forms HRu 4 (CO) 12 BH 2 and HRu 6 (CO) 17 B on standing in solution at room temperature. The transformations are also observed upon photolysis of Ru 3 (CO) 9 BH 5 . A crystallographic study of HRu 6 (CO) 17 B has revealed a new structural isomer in which the boron atom resides at the centre of a distorted octahedral Ru 6 -cavity. Ru 3 (CO) 9 BH 5 reacts with Fe(CO) 5 under photolytic conditions to give HRu 3 Fe(CO) 12 BH 2 , in which the iron atom appears to reside exclusively at a wingtip site. This heterometallic cluster deprotonates by loss of the FEHB proton to give [HRu 3 Fe(CO) 12 BH] − and this anion may also be generated by the direct reaction of [Ru 3 (CO) 9 BH 4 ] − with Fe(CO) 5 . Both HRu 3 Fe(CO) 12 BH 2 and [HRU 3 Fe(CO) 12 BH] − are static on the NMR timescale at room temperature. The solution properties of [Ru 3 (CO) 9 BH 4 ] − are reported, and are compared with those of the conjugate acid.

Palladium catalysed [2 + 2 + 1] intramolecular cycloaddition for the preparation of bicyclo[3.3.0]octa-1.5-dien-3-ones from 1,6-diynesElectronic supplementary information (ESI) available: experimental. See http://www.rsc.org/suppdata/cc/b3/b302841k/

Palladium catalysed [2 + 2 + 1] cycloaddition of 1,6-heptadiynes with CO (1 atm) furnishes bicyclo[3.3.0]octa-1,5-dien-3-ones in 30-74% yield.

The insertion of 1-phenyl-1-propyne into the ruthenaborane cluster HRu4(CO)12BH2 and the isolation and molecular structure of 1-phenyl-2,3-dimethylazulene

Photolysis of the tetraruthenaborane butterfly cluster HRu4(CO)12BH2 with 1-phenyl-1-propyne yields the cluster product HRu4(CO)12B(H)C(Ph)CMeH. Interestingly, 1-phenyl-2,3-dimethylazulene has also been isolated from the reaction mixture. The formation of this substituted azulene is an example of a novel cyclodimerisation of the alkyne. The crystal structure of 1-phenyl-2,3-dimethylazulene has been determined.