Hydrochloric Acid → HCID 17803204, compound

Participants

Reaction Steps

19.6 g (0.29 mol) of sodium cyanoborohydride (95%) are added in portions to a solution of 66.8 g (0.29 mol) of 2-hydroximino-3,3-dimethyl-4-(4-fluorophenoxy)-butane in 500 ml of methanol, which is kept at pH 3 with concentrated hydrochloric acid against bromocresol green. When the addition has ended, the pH value is kept at 3 with hydrochloric acid for a further 3 hours and the mixture is then subsequently stirred at room temperature for 16 hours. The reaction mixture is acidified to pH 1 and concentrated in vacuo. The residue is taken up in chloroform/water, the organic phase is separated off and dried over sodium sulphate and the solvent is distilled off in vacuo. 52.3 g (67.1% of theory) of 4-(4-fluorophenoxy)-3,3-dimethyl-2-butyl-hydroxylamine hydrochloride of melting point 99° C. are obtained. ##STR95##

Provenance & Evidence