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OAs(NMe2)3: Synthesis and crystal structure of the arsenic analogue of HMPT

✍ Scribed by JÖRg Lorberth; Reiner Dorn; Sung-Hee Shin; Michael Otto; Werner Massa

Publisher
John Wiley and Sons
Year
1991
Tongue
English
Weight
249 KB
Volume
2
Category
Article
ISSN
1042-7163

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✦ Synopsis

O = A S ( N M ~~) ~ (HMAsT) is obtained in low yields by reacting O=AsC13 with excess HNMe2 or by ozonolysis of A S ( N M ~~) ~; however, it is formed in yields >65% by using (Me3Si)202 and A S ( N M ~~) ~ in hydrocarbon solution. The structure of HMAsT was established by IRIRaman, NMR and mass spectroscopy, and single crystal X-ray structure analysis. The structure determination revealed (sp3C)-H. ao-hydrogen bonding in the solid state. Acid-base reaction by methanolysis affords ionic [Me2NH2] [O2As(0Me),] while iodide is oxidized to iodine.

Hexamethylphosphortrisamide (HMPT), O=P-(NMe2)3, is, as a consequence of the pioneering work by Michaelis [ l ] , relatively easy to obtain by aminolysis of phosphorus oxychloride (Equation 1); the versatility of HMPT as a reagent has been demonstrated, for example, by H. Normant [ 2 ] in a review article.

0=PCl3 + 6 HNMe2 --+ O=P(NMe2I3 + 3 H2NMe2Cl (1)

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