Darstellung und Eigenschaften von S ‐(Trifluormethyl)polysulfanmonosulfonaten CF 3 S x SO 2 M [ x = 1, M = OH, NH 40 O, 1/2 HgO 2 , (CH 3 ) 3 SiO, (CH 3 ) 2 N, NH 2 ; x = 2, M = NH 4 O]

Synthesis and Properties of S ‐(Trifluoromethyl)polysulfanemonosulfonates CF 3 S x SO 2 M [x=1, M = OH, NH 4 O, 1/2 HgO 2 , (CH 3 ) 2 N, NH 2 ; x =2, M = NH 4 O]* Hydrolysis of CF 3 SNSO with 2 equiv. of H 2 O provides [NH 4 ][CF 3 SSO 3 ] ( 1 ), which on treatment with chlorine gives CF 3 SCl and [NH 4 ][ClSO 3 ]. Trifluoromethyl thiosulfates are synthesized from Hg(SCF 3 ) 2 and ClSO 2 M [M = NH 4 O, (CH 3 ) 3 SiO ( 2 ), (CH 3 ) 2 N ( 3 ), NH 2 ( 4 )]. Insertion of SO 3 into Hg(SCF 3 ) 2 provides Hg[CF 3 SSO 2 O] 2 ( 6 ). Similarly, S ‐(trifluoromethyl)thiosulfuric acid ( 5 ) is obtained from CF 3 SH and SO 3 . New preparations for CF 3 S X NSO ( x =1, 2) are described. These compounds are formed either from Hg(NSO) 2 or (CH 3 ) 3 SiNSO and CF 3 S x Cl in good yields. CF 3 SSNSO ( 8 ) reacts with water to give [NH 4 ][CF 3 SSSO 3 ] ( 9 ). A 1:1 adduct ( 10 ) is obtained from CF 3 SNSO and AsF 5 . A preliminary X‐ray structure investigation proved that AsF 5 is coordinated to the oxygen atom. Some reactions of [NH 4 ][CF 3 SSO 3 ] and CF 3 SSO 2 OSi(CH 3 ) 3 are mentioned.