Hydrochloric Acid → HCID 19888723, compound

Participants

Reaction Steps

A solution of the compound obtained in step (i) above (3.2 g, 0.0092 mol) in anhydrous tetrahydrofuran (65 ml) is heated to the reflux temperature under nitrogen atmosphere and a 10M solution of borane-methyl sulfide (2.8 ml, 0.028 mol) and anhydrous tetrahydrofuran (10 ml) are then added thereto. The mixture is refluxed for 4 hours, methanol (30 ml) is slowly added thereto and refluxing is prolonged for an additional hour. lN HCl (60 ml) is then added thereto and the mixture is refluxed for 1 hour, and concentrated under reduced pressure. The residue is taken up in ethyl acetate, the organic solution is washed with ammonium hydroxide and then with water, dried over sodium sulfate, filtered and concentrated to dryness under reduced pressure affording a solid which is washed with isopropyl ether (2.3 g). M.p. 150°-153° C.

Provenance & Evidence