Hydrochloric Acid → HCID 13645764, compound

Participants

Reaction Steps

The ester from Example 2 (9.6 gm) in a mixture of 135 ml n-BuOH and 45 ml 45% KOH (aq) was refluxed with good stirring for 75 min., allowed to cool, and acidified with 68 ml conc. HCl. The reaction mixture was transferred to a 1 liter round bottom flask, rinsing and diluting with 40 ml n-BuOH. The mixture was concentrated to about 350 ml, cooled, and the KCl filtered off. The filtrate was concentrated to dryness then warmed and shaken with 40 ml acetonitrile, filtered and rinsed with acetonitrile (5 ml). The filtrate was cooled, seeded and the product allowed to crystallize. Wgt.=4.1 gm, m.p.=144°-145°. A second crop was obtained from the filtrate, Wgt.=1.1 gm.

Provenance & Evidence