Detection of Aryl(vinyl)nitroxides by ESR Spectroscopy

✍ Scribed by Doz. Dr. H. G. Aurich; Dr. F. Baer

• Publisher: John Wiley and Sons
• Year: 1967
• Tongue: English
• Weight: 216 KB
• Volume: 6
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.196710801

✦ Synopsis

It is thus proved that oxophosphoranesulfenyl chlorides P(0)SCI and esters of tervalent phosphorus acids P-0-R(H) give first the thiol form (3) of the mono-\ < thiopyrophosphate system [31. 2.37 2.37 2.33 2.62 2.64

Synthesis of bis(5,5-dimethyt-2-oxo-l,3,2-Pv-dioxaphos-phorinanyI)sulfide ( I ) :

A solution of sulfur dichloride (2.06 g, 0.02 mole) in benzene (20 ml) was added dropwise to a solution of 5,5-dimethyl-2oxo-1,3,2-dioxaphosphorinane (3) (6.0 g, 0.04 mole) and triethylamine (4.04 g, 0.04 mole) in benzene (50 ml) at 20 to 30°C (ice cooling). The whole was stirred at room temperature for 1 h and the crystal mass was filtered off with suction, washed with benzene (2 x 50 ml) and water (2 x 50 ml), and dried. Yield, 4, O g; m.p. 162-167 "C; m.p. 185-188 "C after recrystallization from benzene/chloroform.