FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for preparing acetylenic alcohols by continuous method. Method involves condensation of ketones of the general formula: R1-CH2COCH2-R2 with acetylene at temperature about 20-50 C and under pressure about 10-30 kg/cm2. Anion-exchange resin is used as a catalyst with groups of quaternary ammonium hydroxide with strong basicity in proton solvent. Feeding reaction mixture is carried out with hour volume rate from 0.1 to 5.0 h-1. Reaction mixture contains acetylene, ketone and solvent taken in the mole ratio = 1.0 : (0.2- 3.0) : (1.0-4.0), respectively. Ketone comprises substituents R1 and R2 that can be similar or different and each means hydrogen atom, linear or branched saturated or unsaturated alkyl comprising 1-16 carbon atoms. Preferably, acetylenic alcohol is prepared taken among the group: 2-methylbut-3-in-2-ol, 3,7-dimethyl-oct-6-ene-1-in-3-ol, 3,7,11-trimethyl-dodeca-6,10-diene-1-in-3-ol, 3,7,11,15- tetramethyl-6,10,14-hexadecatriene-1-in-3-ol and 3,7,11,15-tetramethylhexadeca-1-in-3-ol. As ion-exchange resin Amberlite-402 or Amberlite-900, resin AB-17-8 in OH--form is used. Aprotonic solvent is taken among the group consisting of dimethylformamide, dimethyl- sulfoxide and N-methylpyrrolidone. Invention provides carrying out the process under mild conditions with high yields of the end product and minimal amount of harmful waste of production. EFFECT: improved preparing method. 11 cl, 14 tbl, 8 dwg, 14 ex _
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Authors
Dates
2003-11-20—Published
1999-08-24—Filed