P R E P A R A T I O N O F T R I S - ( f i , f l , f i - T R I F L U O R O E T H Y L ) A N T I M O N Y

D I F L U O R I D E

G. G. B e l e n ' k i i , Yu. L . K o p a e v i c h , L . S. G e r m a n , a n d I . L . K n u n y a n t s

UDC 542.91:547:413:546.86'131

It was established that when SbFs(I ) is reacted with CF2=CF2, CF2=CFC1, or CF 2 = CFH at 50~ and a tmospher ic p r e s s u r e the indicated olefins are fluorinated at the double bond with the formation of the cor - responding polyfluoroalkanes

SbFa CF2=CFX ~ CFa--CFuX (X=C1, F, H)

In the case of CF 2 = CH2(II ) it is observed that (1) adds to the double bond with the formation of t r i s - (fi,fi,fi-trifluoroethyl)antimony difluoride (IIl)

CF2=CH~ SbF, (CF3CH~)3SbF~ (II) (III)

The same product was obtained by react ing (1") with (II) in SO 2 solution. Into a solution of 30 g of (1) in 50 ml of liquid SO 2 was passed 12.5 l i ters of (II) at 20 ~ in 4 h. The reaction mixture was poured on ice, and the obtained crysta ls were filtered and recrys ta l l i zed from CClt. We obtained 11.5 g of (III), 20% yield, mp 72 ~ Found: C 17.73; H 1.46; F 51.21%. C~FllHGSb. Calculated: C 17.60; H 1.46; F 51.10%. 19F NMR spectrum: tr iplet , 5 - 2 1 . 5 ppm (from CF3CO2H as the external standard), JCF3_ H = 11.2 Hz. PMR spec- t ram: quartet , 5 3.34 ppm (relative to HMDS as the external standard), I H _ C F 3 = 12.2 Hz. Mass spectrum: m/e 389 (M-F~), 325 (-CF3CH2+), 261 (CFsCH2SbF3).

Institute of Heteroorganic Compounds, Academy of Sciences of the USSR. Translated from Izvest iya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 4, p. 983, April , 1972. Original ar t ic le submitted Jan- uary 10, 1972.

�9 1972 Consultants Bureau, a division of Plenum Publishing Corporation, 227 West 17th Street, New York, N. Y. 10011. All rights reserved. This article cannot be reproduced for any purpose whatsoever without permission of the publisher. A copy of this article is available from the publisher for $15.00.

950