VERFAHREN ZUR HERSTELLUNG VON O-SUBSTITUIERTEN HYDROXYLAMMONIUMSALZEN

摘要

Prepn. of a O-substd. hydroxylammonium salt of formula NH2OR.xHX (I) comprises, without isolation of intermediates: (a) reacting acetone with hydroxylammonium sulphate (A) and NaOH to give the acetonoxime of formula (II); (b) reacting (II) with NaOH and removing water completely; (c) treating the suspension of autonoxime sodium salt of formula (III) with an alkylating agent of formula RY (IV) at 0.5-15 bar and upto 140 degrees C, with addition of phase transfer catalysts to give the autonoxime ether of formula (V); and (d) treating (V) with the acid HX to give (I). All the steps (a)-(d) are carried out in a single, nonpolar, aprotic solvent. R = 1-6C alkyl or 2-6C alkenyl, both opt. halo substd.; X = Cl or Br; Y = leaving gp.