Methanol → HCID 59180418, compound

Participants

Reaction Conditions

Reaction Steps

To a cooled (0° C.) solution of 29 (6.19 g; 37.69 mmol) in anhydrous dichloromethane (160 mL) was added chlorosulfonic acid (3.0 mL; 45.22 mmol) dropwise. After addition as complete, the reaction was stirred at 0° C. for an additional 30 minutes, allowed to gradually warm to room temperature and further stirred overnight. The reaction mixture was concentrated under reduced pressure to about 500 mL and washed with aqueous hydrochloric acid (20 nm; 20N). The organic layer was separated and dried over magnesium sulfate which resulted in formation of a white precipitate. Methanol (200 mL) was added to dissolve the precipitate. The organic solution was filtered and concentrated under reduced pressure to yield the title compound as a purple solid (12.07 g).

Provenance & Evidence