Hydrochloric Acid → HCID 11790499, compound

Participants

Reaction Steps

21.6 g of the ester obtained in (A) was dissolved in 200 ml of tetrahydrofuran, and at room temperature, 100 ml of methanol and then 40 ml of a 10% aqueous solution of sodium hydroxide were added. The mixture was stirred for 1 hour. The reaction mixture was adjusted to a pH of about 4 with cold hydrochloric acid, and concentrated. To the residue were added 300 ml of chloroform and dilute hydrochloric acid. The aqueous layer was adjusted to pH 2, and the chloroform layer was separated. The chloroform layer was washed with an aqueous solution of sodium hydrogen carbonate and also with water, and the solvent was evaporated. Recrystallization of the residue from ethyl acetate-hexane gave 9.2 g (yield 38.0%) of the desired product as colorless prisms having a melting point of 129.0° to 130.5° C.

Provenance & Evidence