反应详情

To a solution of the 2-methyl-6-nitro-benzoic acid (5.6 g, 30.9 mmol, 1.0 eq, Aldrich) and acetone (100 mL) was added crushed K2CO3 (21.4 g, 154.6 mmol, 5 eq) and MeI (9.6 mL, 154.6 mmol, 5.0 eq.). The reaction was heated to reflux for 15 h then cooled to RT, filtered and concentrated in vacuo. The filtrate was dissolved in EtOAc, washed with H2O and brine, dried (MgSO4) and concentrated in vacuo to give the desired compound as a reddish-brown oil which upon standing at RT crystallized as tan needles.

1. temperatureThe reaction was heated
2. temperatureto reflux for 15 h
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. dissolutionThe filtrate was dissolved in EtOAc
6. washwashed with H2O and brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo