Process for the preparation of hydrocarbyl halides
A technology of halides and metal halides, applied in chemical instruments and methods, tin organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of reduced economic benefits, expensive, bulky and difficult to use, and achieve Fast and safe operation, low cost and good yield effect
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Embodiment 1
[0050] Tributylamine (63.6g, 0.34mol) was placed in a 500ml round bottom flask with a stirrer, thermometer socket and condenser. Tin tetrachloride (89.7g, 0.34mol) was slowly added over 1 hour under stirring conditions. The reaction temperature rose from 29°C to 65°C. After the addition is complete, the reaction mass is heated to 100°C under stirring, and then cooled to room temperature. Preparation of dimethyl tin dichloride
Embodiment 2
[0052] The catalyst prepared above (145 g) was placed in a 1 liter stainless steel autoclave, and then tin pellets (200 g, 1.68 gm-atom (mol)) were added. Fill the autoclave with nitrogen to expel the air and release the nitrogen into the air. Connect the methyl chloride cylinder to the reaction vessel. Maintain the temperature of the cylinder by placing it in a hot water bath. The mixture of catalyst and tin was heated to 185°C under stirring, and methyl chloride was introduced until the pressure reached 120 psi. Through the pressure drop in the reaction vessel, it was observed that the reaction started immediately. When the pressure drops to 100 psi, methyl chloride is introduced again until the pressure reaches 120 psi. Continue this step until no pressure drop is observed, indicating that the reaction is complete (330min). After cooling the reaction to about 85°C, the excess methyl chloride was slowly discharged. Fill with nitrogen and discharge excess. This ensures t...
Embodiment 3~10
[0054] The steps of Example 2 were repeated using different catalysts, and the preparation of the catalyst was as described in Example 1. When a complex between phosphine and tin tetrachloride is used, the amine is replaced by phosphine and all other reaction conditions are similar. The results are shown in Table 1.
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