Acetyl chloride → HCID 19742604, compound

Participants

Reaction Steps

In 1.6 l of methylene chloride were dissolved 168 ml of acetyl chloride and 315 g of aluminum chloride. While cooling the resulting solution with ice, 400 g of the compound (7-C) obtained above was added thereto. The mixture was stirred at room temperature for one hour. The reaction mixture was then poured into 10 l of ice water, and the mixture was stirred for one hour. The methylene chloride layer was separated, washed twice with water and concentrated under reduced pressure. To the concentrate, there was added 2 of acetonitrile. The mixture was heated under reflux for one hour and then left to stand to cool it to room temperature. The resulting crystal was recovered by filtration to obtain 383 g of the compound (7-D). Yield: 93%.

Provenance & Evidence