Water → HCID 23520109, compound

Participants

Reaction Steps

The product of step B (25 mg, 24 umol) in methanol (3 mL) was added to 10% palladium on carbon (14 mg) in methanol (3 mL) under nitrogen in a Parr bottle. It was hydrogenolyzed at 50 psi for 180 min, filtered through Celite, rinsed with methanol, and concentrated to afford a viscous oil. This was redissolved in 1:1 water/acetonitrile containing 0.1% TFA (nmL) and lyophilized (1:1 acetontrile/water/0.1% TFA) to afford the product as a white powder (29 mg, 100% yield) which analyzes for 2 equal peaks by HPLC (4.6×150 mm Zorbax C-18, 1 mL/min; Water/90% acetonitrile/0.1% trifluoroacetic acid, 2-100% B over 14 min) Rt=9.78 and 10.14 minutes. LRMS (ES): 1054.5 ([M+H]+, 10%) 527.8 ([M+2H]+2, 100%); identical for each peak. This was not further purified but taken into the next step as a mixture of two diastereomers.

Provenance & Evidence