Hydrogen Bromide → HCID 68828061, compound

Participants

Reaction Steps

To a 25 mL single-necked flask was added 180 mg (0.65 mmol) of 9 and 5 mL of glacial acetic acid and 5 mL of 48% HBr. This mixture was heated under reflux for 18 h and then cooled to room temperature. The pH was then adjusted to 10 with cooling with 50% NaOH. This mixture was extracted 3× with methylene chloride. The organic extracts were dried (Na2SO4), and concentrated under reduced pressure to give 0.17 g (99%) of crude product as a white solid. Purification by chromatography on alumina using 15% ethyl acetate/hexane gave 0.140 g (83%) of desired product as a crystalline white solid.

Provenance & Evidence