Methyl iodide → HCID 86658458, compound

Participants

Reaction Conditions

Reaction Steps

Potassium carbonate (177 mg, 1.28 mmol), DMF (2 ml) and MeI (60 ml) were added to the compound (230 mg, 0.65 mmol) obtained in Step 1. The mixture was stirred at 40° C. for 6 hours. Potassium carbonate (44.3 mg) and MeI (40 μL) were supplemented and stirred overnight. After the solvent was removed by distillation, the purification step A was applied to give the crude product of 3-{methyl[(2-nitrophenyl)sulfonyl]amino}benzenesulfonic acid (160 mg). This crude product (144 mg, 0.39 m ml) was dissolved in DMF (3 ml), and cesium carbonate (126 mg, 0.39 mmol) and thiophenol (40 μl, 0.39 mmol) were added to the solution. The mixture was stirred at 50° C. overnight. After the solvent was removed by distillation, the purification step A was applied to give the crude product of 3-(methylamino)benzenesulfonic acid (84.1 mg).

Provenance & Evidence