反应详情

A suspension of 3D (50 mg, 0.142 mmol) and palladium hydroxide (20% wt of Pd) on carbon (50 mg) in EtOAc (5 mL)/methanol(2 mL) was stirred under a hydrogen balloon for 5 hours, then filtered via a pad of Celite. The filtrate was concentrated under reduced pressure. The resultant residue was purified by silica gel column chromatography eluting with 2.0 M NH3 in MeOH/CH2Cl2 (3:97 ratio) to give the desired product, which was further purified using preparative HPLC to give the title compound as a TFA salt (15 mg, 22% yield). LC/MS (method A): retention time=2.75 min, (M+H)+=355.

1. filtrationfiltered via a pad of Celite
2. concentrationThe filtrate was concentrated under reduced pressure
3. customThe resultant residue was purified by silica gel column chromatography
4. washeluting with 2.0 M NH3 in MeOH/CH2Cl2 (3:97 ratio)