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In a study with v a ria tio n of th e y lid -n itro b en zen e r a tio and subsequent treatm ent with a ir , th e optimum re a c tio n conditions fo r the m ethylation of nitrobenzene w ith dimethyloxosulfonium y lid were found to be an 8-fo ld molar excess of m ethylid over n itrobenzene,and i n i t i a l re a c tio n fo r 15 m inutes in an atmosphere of n itro g en ,fo llo w ed I X by passing a ir through th e re a c tio n m ixture fo r 5 hours p rio r to work-up. With th ese experim ental co nditions th e n itro to lu e n e y ie ld was in creased from 17$ to 40-50$, d ia lk y la tio n was observed, and e s s e n tia lly no nitrobenzene was recovered.