FIELD: organometallic synthesis.
SUBSTANCE: invention relates to a method of producing tetrakis(dimethylamino)titanium of electronic quality. Method is carried out by reacting dimethylamine and a titanium (IV) salt. Titanium disulphide is obtained in reaction volume by introducing titanium tetrachloride into cooled tetrahydrofuran, reactor cooling temperature is set, followed by passing through the obtained hydrogen sulphide solution. Further, a tertiary amine is added to the reaction mixture at a temperature below minus 8 °C and holding the reaction mass while stirring for at least 4 hours, followed by distillation of tetrahydrofuran from the reaction mass, formed titanium disulphide is diluted with anhydrous benzene and dimethylamine is added with heating the reaction mixture to temperature of 80 to 85 °C, distillation of benzene and obtaining tetrakis (dimethylamino) titanium, which is separated from the reaction mixture by distillation under high vacuum at temperature of 70 °C.
EFFECT: obtaining tetrakis(dimethylamino)titanium of electronic quality with high output (up to 93%), which does not require additional purification.
7 cl, 1 dwg, 5 ex
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Authors
Dates
2024-08-19—Published
2023-12-13—Filed