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

Active Publication Date: 2015-02-18
QUZHOU LANRAN NEW MATERIAL CO LTD
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Problems solved by technology

More heat will be released during hydrolysis, and the dichloromethane added after the reaction will have a greater risk of "bumping" because of its low boiling point

Method used

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  • Method for preparing 1-chlorine-2-(dichloro(benzene)methyl) benzene solution

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preparation example Construction

[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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Abstract

The invention discloses a method for preparing a 1-chlorine-2-(dichloro(benzene)methyl) benzene solution. As to an important precursor 1-chlorine-2-(dichloro(benzene)methyl) benzene required for manufacturing solid-phase synthetic resin of 2-chlorine trityl alcohol, reflux reaction on2-Chlorobenzophenone and excessive phosphorus pentachloride is carried out by adopting dichloroethane as a reaction solvent; then a reaction liquid is slowly put into an ice water mixture to hydrolyze and an organic phase is washed with running water for a plurality of times; an organic phase is obtained by dividing the liquid; and a drying agent is added to dewater, so as to obtain the 1-chlorine-2-(dichloro(benzene)methyl) benzene solution. The solution has very low byproduct content and is of light color; and the method is simple and efficient; and the solution can be directly used as the reaction liquid for producing 2-chlorine trityl alcohol resin. Therefore, the material is low in cost; and the resin product is good in color and luster and appearance, and good in swelling properties.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis of fine chemicals, in particular to a preparation method of 1-chloro-2-(dichloro(phenyl)methyl)benzene solution. Background technique [0002] Since Merrifield founded Solid Phase Peptide Synthesis (SPPS) technology in 1963, it has been increasingly used in the research and development of bioactive peptides due to its advantages of simple operation, less by-products, and high purification efficiency. , especially widely used in the actual production of medicinal short peptides. In the solid-phase synthesis of polypeptides, 2-chlorotrityl chloride (2-Chlorotritylchloride, referred to as 2-CTC) resin can effectively inhibit side effects such as racemization and diketopiperazine formation due to milder reaction conditions than other resins. The occurrence of the reaction and the high purity of the product have been widely used in the industrial production of various polypeptide drugs (such...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C25/02C07C17/18C08F12/08C08F8/18
Inventor 雷引林罗云杰殷锦邓承毅
Owner QUZHOU LANRAN NEW MATERIAL CO LTD
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