Ethyl Acetate → HCID 12878332, compound

Participants

Reaction Steps

7 g of LiAlH4 are added in portions at 0° under an inert gas atmosphere to 16 g of (5-chloro-4- cyclohexyl-2-methoxyphenyl)-acetic acid methyl ester in 350 ml of dry tetrahydrofuran. Stirring is then effected for 18 hours at 22° . 20 ml of ethyl acetate are carefully added in drops so as to destroy the excess LiAlH4. The mixture is then poured onto a solution of NH4Cl in ice water, acidified with 2N H2SO4 and extracted three times with acetic ester. The organic phases are washed with water, dried over Na2SO4 and concentrated. The residue is chromatographed on 250 g of silica gel. The product, which is extracted with methylene chloride, is distilled in a bulb tube. M.p. 78°-79°.

Provenance & Evidence