Diethyl Ether → HCID 53690970, compound

Participants

Reaction Steps

To 30 ml of abs. ether cooled to 3° is added under nitrogen 1.14 g (0.03 mole) of lithium aluminium hydride, and there is then added dropwise at 5°-10° with stirring, within half an hour, a solution of 5.4 g (0.02 mole) of 5-chloro-2-(2-thienylthio)-benzoic acid (produced according to Swiss Patent Specification No. 405,354; C.A. 66, P 2550e) in 45 ml of abs. ether. After completion of the dropwise addition, the mixture is refluxed for 16 hours; and there is thereupon slowly added dropwise at 3°-7° 5 ml of water. The occurring precipitate is filtered off with suction, and subsequently well washed with ether. The filtrate is concentrated in vacuo, and the residue is recrystallised from carbon tetrachloride to yield 5-chloro-2-(2-thienylthio)-benzyl alcohol having a melting point of 95°-96°.

Provenance & Evidence