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and (ii) by the absence of any shift of the 19F-NMR signal of the terminal CF21 group of (1) in DMF solution after saturation with SOz, ruling out activation of (1). Complexes (2) are most probably formed by oxidative addition of (1) to an initially formed M0(SO2) complex, to give a solvated (RMI) species and insertion of SOz into the M--C bond.The postulated insertion reaction of SO2 into a perfluoroalkyl-transition metal bond appears unusual[41. However, it could be accomplished with the model compound ( 90% yieldThe synthesis of sulfinato complexes is not limited to (1) but is also possible with other halides. The products are sometimes highly labile and could not all be characterized. The is added dropwise to a stirred suspension of Fe powder['J (27.9 g, 0.5 mol) in DMF (750 ml) over 3 h with simultaneous introduction of SO2 (64 g, 1.0 mol). The mixture is kept below 25 "C, and first turns green and then yellowish-brown. After stirring for 48 h, it is filtered and as much DMF removed as is possible at 0.1 torr and a maximum temperature of 30 "C. The distillate contains ca. 5 g of COF13H. The residue is cooled to -20°C for several days; the crystal slurry is filtered under suction and the crystals dried in uacuo (yield 378 g). (2b, c) can be prepared similarly.

The complete manuscript of this communication appears in: Angew. Chem. Suppl. 1982, 1201. DOI:

Professor Klaus Weissermel zum 60. Geburtstag gewidmetDer Triazolylessigester 1 kann rnit Ameisensaure-ethylester formyliert werdenl'l. Durch Ansauern des Natriumenolats 2 erhalt man die 3-Hydroxy-2-( 1,2,4-triazol-1-y1)acrylsiureester 4 in guten Ausbeuten. Mit Chlortrimethylsilan reagiert 2 zum Trimethylsilylenolether 3, dessen Hydrolyse, die schon beim Absaugen vom gebildeten Natriumchlorid in Gegenwart von Luftfeuchtigkeit eintritt, in quantitativer Ausbeute ebenfalls 4 ergibt.