Methanesulfonic Acid → 100539-95-5

Participants

Reaction Conditions

Reaction Steps

Methanesulfonic acid (6.26 g, 0.065 mol) was added in one portion to a slurry of the compound prepared in Step 1 above (11.9 g, 0.044 mol) in toluene (300 mL) at 0° C. After 5 minutes, the mixture was heated to reflux for 18 hours, allowed to cool to 0° C., filtered, and the residue washed with cold toluene (50 mL at 5° C). The solid was dried in vacuo, suspended in water (200 mL), and made basic with ammonium hydroxide (0.1M) while stirring vigorously. The resulting solid was filtered, washed with water, dried in vacuo to give 7.2 g of a white solid.

Provenance & Evidence