METHOD FOR PREPARING TERTIARY ADAMANTANE ALCOHOL ACRYLATE AND METHACRYLATE Russian patent published in 2003 - IPC

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to the improved method for preparing acrylates and methacrylates of tertiary alcohols of adamantine order that are used as parent compounds for polymeric materials for 193 nm laser microlithography in making semiconductive devices. Method involves interaction of adamantanone-2 with alkylmagnesium halide followed by successive addition to reaction mixture of tertiary organic base, derivative if acrylic or methacrylic acid and water and the following filtration of precipitate of formed inorganic salts and isolation of end compounds. Method involves usage of alkylmagnesium halides of the general formula AlkMgHal wherein Hal is J, Br, Cl; Alk is -CH₃,C₂H₅,n-C₃H₇,i-C₃H₇,n-C₄H₉. Bases taken among the group: triethylamine, tributylamine, diethylbenzylamine, pyridine, 5-(N,N-dimethylamino)- pyridine or N, N-dimethylaniline are used tertiary organic base. Reaction is carried out at temperature 0-10 C in the presence of anhydrous metal halide taken among the group: TiCl₄,AlHal₃,MgHal₂,FeHal₃,SnCl₄ and the following interaction with anhydride or halogen-anhydride as derivative of acrylic or methacrylic acid at 0-80 C in the weight ratio adamanatanone-2 : alkylmagnesium halide : metal halide : organic base : derivative of acrylic or methacrylic acid = 1 : (0.7-2.4) : (0-1.0) : (0.06-2.0) : (0.7-3.0), respectively. Amount of added water is 0.17-0.74 weight part per the parent adamantanone-2. Invention provides to elevate selectivity, to simplify technological process and to reduce amount of flows. EFFECT: improved preparing method. 10 ex