Synthesis and X-Ray Crystal Structure of an Annelated Spirophosphorane

Abstract

Reaction of the 2-azidoalcohol 1 with 2-phenyl1-1,3,2-dioxaphospholane leads to a 4:1 mixture of the pentacoordinate phosphorane 3 and the diazadiphosphetidine 4. In solution, these compounds are in equilibrium, presumably involving the not detectable iminophosphorane 2. A single X-ray analysis carried out on 3 proves the structure of this type of compound which has been postulated earlier as intermediate in the synthesis of aziridines from azidoalcohols^1,2     

New Organotin Compounds Including a Tin–Zinc Bond

Abstract

The reaction of dialkyltinhydrides with dialkylzinc results in a tin metal bond formation. Crystal structures of 1,1,1,2,3,3,3-hepta-phenyl-2-(ethylzincio)tristannane *TMEDA 1, 1,1,2,2,3,3,4,4-octaphenyl-1,4-(ethylzincio)tetrastannane*2TMEDA 2, and triphenyl(phenylzincio)stannane*TMEDA 3 could be obtained.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.

GRAPHICAL ABSTRACT     

Structures and properties of solvated and unsolvated isopropyl functionalised calix[4]arenes

The tetra-isopropyl ethers of calix[4]arene and p-t-butylcalix[4]arene have been isolated in the cone conformation, and structurally characterised as chloroform solvates. Thermogravimetric analysis demonstrated that the parent isopropylcalix[4]arene solvate is significantly more stable than the p-t-butylcalix[4]arene analogue, retaining the solvent up to a temperature of 125°C. It was found that the calix[4]arene ether sublimes at atmospheric pressure, and solvent-free crystals appropriate for structure determination were produced at reduced pressure. The p-t-butylcalix[4]arene ether was also isolated without solvent in the lattice, but in this case the calixarene was crystallised from acetone, as sublimation did not produce crystals of sufficient quality.