Stirred 10.25 g ClO3F in 300 ml MePh at -70 Deg, under N, was treated with 160 ml 0.41M triphenylphosphonium methylide to give 98% [Ph3P+CH2F]ClO3- (I), m. 131-4 Deg (CH2Cl2-AcOH-EtOAc). Satd. 1 equiv. I in Me2CO treated with 1.25 equivs. NaI in Me2CO gave ...
1969