Methanesulfonic Acid → HCID 178505362, compound

Participants

Reaction Steps

The compound obtained in Example 5 (16.7 g, 39.8 mmol) was suspended in MeOH/CH2Cl2 (1/4 v/v, 350 mL) and stirred at 50 until the compound obtained in Example 5 was dissolved clearly. The mixture thus obtained was cooled to 0 and methylsulfonic acid (2.9 mL, 43.8 mmol, 1.3 eq, Aldrich 471356) was added thereto at 0. The resulting mixture was evaporated in vacuo to remove solvent. The resultant solid was suspended in absolute EtOH (100 mL) and the suspension was stirred at 90 to dissolve solid clearly. The resulting mixture was cooled to 0 and stirred at 0 for 2 hrs. The solid thus produced was filtered off, washed with absolute EtOH (100 mL), and dried under high vacuum to obtain the title compound.

Provenance & Evidence