- Crystal Structures and Phase Transitions of 3-Chloro-2,2-bis(chloromethyl)propionic Acid-1 and 1,3-Dichloro-2,2-dimethylpropane
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The crystal structure of 3-chloro-2,2-bis(chloromethyl)propionic acid-1 was determined from single crystal data. The compound crystallizes in the acentric monoclinic space group P21. Lattice constants at T = 304 K are a = 6.961(1) A, b = 9.979(2) A, c = 12.0569(3) A β= 94.01(2)°. Structure refinement on 1736 independent reflections yielded R = 0.041. Two molecules are interconnected by hydrogen bridges to form dimers. Thermal analysis and temperature dependent X-ray and IR-measurements gave no indication of a phase transition in the range 150 K I→II = 194.3 K, with a plastic cubic phase in the range 194.3 K (200 K) = 2.6769 × 10-4 K-1. The entropy at the melting point Tm = 259.1 K and at the solid-solid phase transition TI→II = 194.3 K is rather low giving strong evidence of a plastic phase. Powder X-ray diffraction pattern in the ordered phase at T = 160 K gave indication of monoclinic symmetry with a = 12.27 A, b = 10.86 A, c = 10.68 A, β = 111.8°. Temperature dependent infrared measurements revealed the conformation of the molecule.
- Goetze, Astrid,Buhrmester, Claudia,Svoboda, Ingrid,Fuess, Hartmut
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p. 443 - 456
(2007/10/03)
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- A novel rearrangement reaction conversion of 3-(chloromethyl)azetidin-2-ones to azetidine-3-carboxylic acid esters
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Transformation of 3-(chloromethyl)azetidin-2-ones to azetidine-3-carboxylic acid esters is described. The readily available 3-(chloromethyl)azetidin-2-ones rearranged in good yields to azetidine-3-carboxylic acid esters on treatment with alkoxides. An alternative ring opening - ring closure procedure is also identified.
- Bartholomew,Stocks
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p. 4795 - 4798
(2007/10/02)
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