Boron tribromide → HCID 70242181, compound

Participants

Reaction Steps

To a solution of the compound of Example 105 (0.34 g) in dichloromethane (20 ml ) at —78° C. was added boron tribromide (2.6 ml ). the reaction was allowed to warm to room temperature. After 2 hours, the reaction was quenched with ammoniacal methanol solution and the solvent removed under reduced pressure. The crude material was purified on silica eluting with 80:20:3 dichloromethane:methanol:ammonium hydroxide. The product containing fractions were pooled and the solvent removed under reduced pressure. The solid was purified further using MCI gel chromatography eluting with a solvent gradient of 100:0 to 0:100 water:methanol. The product-containing fractions were concentrated, a small volume of concentrated ammonium hydroxide added and the solution freeze-dried to give the title compound (0.11 g).

Provenance & Evidence