Trifluoromethanesulfonyl chloride → HCID 13826402, compound

Participants

Reaction Steps

4,6-Dichloro-7-hydroxyindan-1-one (21.71 g., 0.1 mole) was dissolved in DMF (80 ml) in a dry apparatus under nitrogen. Trifluormethanesulfonylchloride (21.60 g., 0.128 mole) was added with stirring, slowly, dropwise over a 20 minute period with occasional cooling to keep the internal temperature below 30° C. After the addition was complete, the reaction was stirred at room temperature for 30 minutes, then poured into ice-water with swirling. The green crystals were collected, washed with water, sucked dry, then dried in a vacuum oven at 50° C. to give 32.7 g. of the title compound mp 96°-100° C. Recrystallization from hexanes gave 22.4 g., mp 96°-98° C. A sublimed sample had mp 90°-96° C.

Provenance & Evidence