Phloroglucinol → HCID 9968839, compound

Participants

Reaction Steps

39.8 g (0.33 mol) of methanesulfonic acid chloride were added dropwise at 0° C. within the course of 30 minutes to a solution of 12.6 g (0.10 mol) of phloroglucinol and 101 g (1.0 mol) of N-methylmorpholine in 200 ml of dry tetrahydrofuran in such a way that the temperature did not rise above 10° C. After the dropwise addition, the ice bath was removed, and the mixture was warmed to room temperature and stirred for 2 hours at this temperature. The mixture was then slowly added dropwise with continuous stirring to 3 l of ice water, and the resulting precipitate was filtered off with suction and washed until neutral with water. After drying, this gave 32.9 g (91%) of a colorless powder of melting point 145 to 149° C. Recrystallization from an isopropanol/acetone solvent mixture gave colorless, highly light-refracting platelets of melting point 150° C.

Provenance & Evidence