Reactions of dithioxo‐1,3,2λ ⁵ ,4λ ⁵ ‐dithiadiphosphetanes with arsenic derivatives containing the As‐O, As‐S, and As‐N bonds

Disproportionation of Diethylarsanyl N,N-Diethyl(3,5-di-tert-butyl-4-hydroxyphenyl)-phosphonamidodithioate

“…In particular, diorganylphosphanyl N,N-dialkylarylphosphonamidodithioates with the R 2 N3P(S)S3P< fragment, regarded as the products of insertion of monomeric fragments of 2,4-diaryl-1,3,2,4-dithiadiphosphetane 2,4-disulfides into the N3P bond of aminophosphines, transform under heating to the sulfides of the starting aminophosphines and the products of condensation of arylmetadithiophosphonates [1]. We have previously prepared diorganylarsanyl N,N-dial-ÄÄÄÄÄÄÄÄÄÄÄÄ kylarylphosphonamidodithioates containing an R 2 N3 P(S)S3As< fragment by the reactions of 2,4-diaryl-1,3,2,4-dithiadiphosphetane 2,4-disulfides with aminoarsines [2]. We found that, contrary to the compounds with the R 2 N3P(S)SP< fragment, diethylarsanyl N,Ndiethyl(3,5-di-tert-butyl-4-hydroxyphenyl)phosphonamidodithioate I disproportionates at 70oC within 1 h to form crystalline bis(diethylarsanyl) 3,5-di-tert-butyl-4-hydroxyphenylphosphonotrithioate II.…”

“…Complete results of the X-ray diffraction analysis will be reported later. N,N-diethyl(3,5-di-tert-butyl-4-hydroxyphenyl)phosphonamidodithioate I prepared from 4.1 g of dithiaphosphetane disulfide IV and 2.8 g of diethyl(diethylamino)arsine in 10 ml of anhydrous benzene at~20oC similarly to the procedure from [2] was heated for 1 h at 70oC. The resulting mixture was filtered, and the filtrate was evaporated for 2 h in a vacuum (0.02 mm) to obtain 1. b.…”

“…The structure of II was comfirmed by an independent synthesis from 2,4-bis(3,5-di-tert-butyl-4-hy-: droxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide IV and bis(diethylarsanyl) sulfide V at~20oC for 1 h [reaction (2)]. …”