Hydrochloric Acid → HCID 178471595, compound

Participants

Reaction Steps

Sodium hydride (0.03 g of an 80% dispersion in mineral oil) was added to ethanol (4 ml). After 5 minutes (3S,4R)-4-(3-cyano-2-methylisothioureido)-3,4-dihydro-6-(1-[3-ethoxycarbonylprop-1-yl]-1H-tetrazol-5-yl)-3-hydroxy-2,2,3-trimethyl-2H-benzo[b]pyran (see Example 75) (0.2 g) was added and the mixture was allowed to stand at room temperature for 16 hours. The solution was acidified to pH 3 with 2N hydrochloric acid and then was concentrated in vacuo. The residue was purified by chromatography on silica eluting with dichloromethane containing methanol (2.5%). The product-containing fractions were combined and concentrated in vacuo to give an oil which was triturated with hexane to give the title compound as a foam, 0.09 g. Found: C,57.00; H,6.46; N,19.48; C23H31N7O5.0.1 hexane requires: C,57.35; H,6.60; N,19.83%.

Provenance & Evidence