Water → HCID 11131622, compound

Participants

Reaction Steps

A solution of XXIX (1.1 g, 0.003 mol) in dry THF (10 mL) was added dropwise with stirring at 0°-4° C. to a suspension of LAH (0.14 g, 0.0036 mol) in dry THF (10 mL). The mixture was stirred at room temperature, further cooled, H2O (0.13 mL) added, followed by 10% NaOH (0.2 mL) and finally H2O (0.33 mL). The mixture was stirred at room temperature for 30 minutes, then at 0° C. for 1 hour, filtered and the collected solid, washed with THF, hot EtOH (2x) and CHCl3. The combined filtrates were concentrated to dryness. The residue was triturated with hot absolute EtOH to yield 0.7 g (69%) of XXX; m.p. 243°-4°.

Provenance & Evidence