Potassium Hydroxide → HCID 53856080, compound

Participants

Reaction Steps

To a cold degassed solution of the compound prepared in Example 2 (22.6 g, 64.9 mmol) in EtOH (700 ml) was added 3M KOH (350 ml) dropwise over 30 minutes. When the addition was complete the reaction was warmed to room temperature. After 3 days the reaction was diluted with H2O, Et2O and brine. The layers were separated and the aqueous layer was further extracted with Et2O (2×). The combined Et2O layers were extracted with 0.1M KOH (1×). All of the aqueous basic layers were combined and cooled to 15° C. and acidified dropwise with 3M HCl (aq) (note: do not let the internal temperature rise above 18° C.).

Provenance & Evidence