Method for preparing 1-chlorine-2-(dichloro(benzene)methyl) benzene solution
A technology of benzene solution and methyl), which is applied in the field of preparation of 1-chloro-2-methyl)benzene solution, achieves the effects of good color and appearance, reduced by-product content and excellent swelling performance
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[0014] The preparation method of 1-chloro-2-(dichloro(phenyl)methyl)benzene solution of the present invention comprises the steps:
[0015] 1. Put o-chlorobenzophenone and dichloroethane in a mass ratio of 1:4~8, put them into the reaction kettle, raise the temperature to 55~65°C, and stir until completely dissolved.
[0016] The dosage ratio of dichloroethane and o-chlorobenzophenone is 4~8:1 according to the mass ratio; if the ratio is too low, it is not enough to quickly dissolve o-chlorobenzophenone; if the ratio is too high, unnecessary solvent waste will be caused . The dissolution temperature is controlled at 55~65°C, which is slightly higher than the melting point of o-chlorobenzophenone, but too high a temperature (such as above 65°C) will lead to a more violent instantaneous reaction when the subsequent phosphorus pentachloride is fed, which is difficult to operate unfavorable.
[0017] 2. Put phosphorus pentachloride solid powder with a molar ratio of 1.05~1.2:1 t...
Embodiment 1
[0027] Preparation of 1-chloro-2-(dichloro(phenyl)methyl)benzene solution : At room temperature, inject 1600 milliliters (about 2000 grams) of dichloroethane into a 3-liter three-neck flask, add 400 grams of o-chlorobenzophenone (purity 99%, 1.828 moles), stir, and heat up to 62 ° C in a water bath. After stirring for 20 minutes, the solids were completely dissolved. Slowly add 420 grams of phosphorus pentachloride solid powder (purity 99%, 1.996 mol), slowly heat up to 87°C within 30 minutes, reflux for 12 hours, then gradually cool the reactant to 20°C with a cold water bath. Slowly put the reactants in the three-neck flask into 10 liters of ice / water (mass ratio 3:7) mixture, stir and hydrolyze for 2 hours, the temperature first slowly rises to 57°C, and then falls naturally; stand for 15 minutes, use Separate the lower organic phase with a separatory funnel. Stir and wash the organic phase with tap water 7 times, add 10 liters of tap water each time, stir and wash f...
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