Preparation method of methyl phenyl chlorosilane

[0018] The preparation process of phenylmethyldichlorosilane: in N 2 Or under the protection of Ar, in a 500 mL reaction kettle, add Mg chips (0.28 mol) and solvent (can be taken from ethylene glycol dimethyl ether, 1,4-dioxane, diethyl ether, tetrahydrofuran, methyl tetrahydrofuran , n-butyl ether, methylal or toluene), raise the temperature to 50-100 °C in the kettle, add chlorobenzene (0.25mol) dropwise, after the dropwise addition, the micro-boiling reaction keeps reflux for 2-5 hours, and then stop the reaction , GC detection of by-products ≤ 0.01%. in N 2 Or under the protection of Ar, the MeSiCl 3 (0.25 mol), the solvent was added in a 500ml reaction kettle; after the Grignard reagent prepared above——phenylmagnesium chloride was lowered to normal temperature, it was transferred to the dropping funnel; 5h. The reaction liquid is filtered and washed, and then the solvent is distilled, and the 60-65°C / 300Pa fraction is collected by rectification under reduced pressure,

[0022] in N 2 Or under the protection of Ar, in a 500 mL reaction kettle, add Mg scraps (0.28 mol) and THF (100 mL) in sequence, raise the temperature to 50-66 ℃ in the kettle, add chlorobenzene (0.25 mol) dropwise, after the dropwise addition, micro The boiling reaction was kept under reflux for 2-5h, and the reaction was stopped. The by-product was detected by GC ≤0.01%, and a THF solution of phenylmagnesium chloride was obtained. N 2 Or under the protection of Ar, the MeSiCl 3 (0.25 mol), THF (100 ml) was added to a 500ml reactor. After the phenylmagnesium chloride prepared above is lowered to normal temperature, N 2 Or under the protection of Ar, transfer to the dropping funnel; add the Grignard reagent dropwise, and keep reflux for 2-5 hours after the dropwise addition. The reaction solution was filtered to obtain the magnesium salt (MgCl 2 (THF) 2 ), after washing with THF, directly distill THF, the recovery rate of THF is greater than 95%, rectification under reduced

[0024] in N 2 Or under the protection of Ar, in a 500 mL reaction kettle, add Mg chips (0.28 mol), THF (40 mL) and MePh (80 mL) in sequence, raise the temperature to 50-100 ℃ in the kettle, add PhCl (0.25 mol) dropwise , After the dropwise addition, the slightly boiling reaction was kept under reflux for 2-5 hours, the reaction was stopped, and the by-product was detected by GC ≤ 0.01%, and phenylmagnesium chloride was obtained. N 2 Or under the protection of Ar, the MeSiCl 3 (0.25 mol), THF (100 ml) was added to a 500ml reactor. After the Grignard reagent prepared above dropped to normal temperature, N 2 Or under the protection of Ar, transfer to the dropping funnel; add the Grignard reagent dropwise, and keep reflux for 2-5 hours after the dropwise addition. The reaction solution was filtered to obtain the magnesium salt (MgCl 2 (THF) 2 ), after washing, directly distill THF and MePh, the rate of recovery is greater than 97%, rectification under reduced pressure obtains p