HCID 20155817, compound → HCID 13361807, compound

Participants

Reaction Steps

7.0 g of the compound prepared under (b) are heated under reflux for 8 hours with a mixture of 50 ml of glacial acetic acid/hydrobromic acid (48% strength) in the volume ratio 1:1. After removing the acid in a rotary evaporator, the residue is taken up with methylene chloride/dilute ammonia, and the organic phase is dried and evaporated in a rotary evaporator. The oily residue is chromatographed on silica gel using a mixture of methylene chloride/ethyl acetate in the ratio 19:1. 2.2 g of pale yellow crystals (38% of theory) are obtained, melting point: 122°-123°.

Provenance & Evidence