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• W1608421863 abstract "Abstract Methods for the preparation of cis - 3,5 - dibromo - 4 - oxo - 2,2,6,6 - tetramethylpiperidin -1 - yloxy ( 2b ) and its use as a convenient, selective spin-labelling reagent for amino functions, are described. The crystal and molecular structures of 2b and the bis -nitroxide 4 - [(2',2',5',5' - tetramethylpyrrolin -1 - yloxy) - 3' - carbonyloxy] - 2, 2,6,6 - tetramethyl - 3,5 - dibromo - 3,4 - dehydropiperidin - 1 - yloxy ( 3) [obtained on treatment of 2b with triethylamine] have been determined by conventional heavy-atom techniques. In 2b the individual molecules have mirror symmetry with the bromine atoms equatorial. The N-O bond length is 1.278(5) A, CNC is 125.1(3)° and the N-O bond makes an angle of 24.2° with the CNC plane. In 3 there are two different nitroxide groups. The pyrrolinyloxy ring is virtually planar with a N-O bond length of 1.252(13) A and CNC of 113.1(10)°. The 6 -membered ring exists in a sofa conformation with a pseudoaxial Br atom. Its nitroxide group is tetrahedrally distorted. The N-O bond length is 1.268(15) A, CNC is 121.7(10)° and the N-O bond makes an angle of 16.0° with the CNC plane. The packing of 3 is dictated by a short Br... .O secondary bond of 3.09(1) A, 0.28 A less than the sum of the van der Waal's radii resulting in dimeric units related by a centre of symmetry." @default.
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• W1608421863 date "1977-01-01" @default.
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• W1608421863 title "Preparation, crystal structure and reactions of a new spin-labelling reagent, cis-3,5-dibromo-4-oxo-2,2,6,6- tetramethylpiperidin-1-yloxy" @default.
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• W1608421863 doi "https://doi.org/10.1016/0040-4020(77)88032-0" @default.
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