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Chemically synthetic method for N-chloroformyl imino dibenzyl

A technology of chloroformyl imidodibenzyl and iminodibenzyl: double, which is applied in the field of chemical synthesis of N-chloroformyl imidodibenzyl, can solve the problem that the phosgene reaction cannot be completely quantified and the reaction conditions are harsh , safety hazards and other issues, to achieve the effect of solving the problem of tail gas absorption, high yield and purity, and avoiding difficult storage

Inactive Publication Date: 2007-04-11
ZHEJIANG UNIV OF TECH
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Problems solved by technology

Before the present invention provides, the chemical synthesis method of relevant N-chloroformyl imidodibenzyl is mainly phosgene method, and highly toxic phosgene has brought very big potential safety hazard and environmental disaster to production, and gaseous The phosgene reaction cannot be completely quantified, the reaction conditions are harsh, the requirements for the reaction equipment are high, and the product yield and product quality are low

Method used

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  • Chemically synthetic method for N-chloroformyl imino dibenzyl

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Experimental program
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Effect test

Embodiment 1

[0020] The amount ratio of the feed material is iminodibenzyl: bis(trichloromethyl)carbonate: organic amine catalyst is 1.0: 0.45: 0.05, wherein the organic amine catalyst is pyridine, the organic solvent is tetrahydrofuran, and its consumption is imino 8 times the mass of dibenzyl.

[0021] In a 250mL three-necked flask with mechanical stirring, reflux condenser (with tail gas absorption device), and a thermometer, add 19.26g (100mmol) of iminodibenzyl, bis(trichloromethyl)carbonate 13.35g (45mmol) , pyridine 0.395g (5mmol) and 154g tetrahydrofuran, open mechanical stirring, treat that solid dissolves completely, be heated to tetrahydrofuran reflux temperature, react 12 hours, monitor reaction process with HPLC during the reaction (mobile phase: acetonitrile: water: tetrahydrofuran=40:50 : 10, C18 silica gel column, flow rate 1.0mL / min). After the reaction was completed, part of the solvent was evaporated under normal pressure to obtain a saturated solution, which was cooled...

Embodiment 2

[0023] The amount ratio of the feed material is iminodibenzyl: bis(trichloromethyl)carbonate: organic amine catalyst is 1.0: 0.40: 0.05, wherein the organic amine catalyst is pyridine, the organic solvent is tetrahydrofuran, and its consumption is imino 8 times the mass of dibenzyl.

[0024] The reaction temperature was THF reflux temperature, and the reaction time was 15 hours. Other operations were the same as in Example 1 to obtain 25.1 g of N-chloroformylimidodibenzyl, with a product yield of 97.2% and a purity of 99.2%.

Embodiment 3

[0026] The amount ratio of feed material is iminodibenzyl: two (trichloromethyl) carbonate: organic amine catalyst is 1.0: 0.35: 0.05, wherein organic amine catalyst is pyridine, organic solvent is tetrahydrofuran, and its consumption is imino 8 times the mass of dibenzyl.

[0027] The reaction temperature was reflux temperature, and the reaction time was 15 hours. Other operations were the same as in Example 1 to obtain 24.8 g of N-chloroformyliminodibenzyl, with a product yield of 96.5% and a purity of 98.8%.

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Abstract

The chemical synthesis process of N-chloroformyl imino dibenzyl includes reaction of imino dibenzyl and bis(trichloromethyl) carbonate as materials in organic solvent at 20-150 deg.c in the action of organic amine catalyst for 2-20 hr; and cooling to crystallize. The material includes imino dibenzyl, bis(trichloromethyl) carbonate and organic amine catalyst in the weight ratio of 1.0 to 0.1-3.0 to 0.001-1.0, and organic solvent in 0.5-20 times the weight of imino dibenzyl. Bis(trichloromethyl) carbonate is one kind of organic reagent with low toxicity, high efficiency and good reaction performance. The chemical synthesis process of the present invention has high yield, product purity and excellent industrial application foreground.

Description

(1) Technical field [0001] The invention relates to a chemical synthesis method of N-chloroformyl imidodibenzyl. (2) Background technology [0002] N-chloroformyl imidodibenzyl is an important pharmaceutical intermediate for the synthesis of carbamazepine and oxcarbazepine. Before the present invention provides, the chemical synthesis method of relevant N-chloroformyl imidodibenzyl is mainly phosgene method, and highly toxic phosgene has brought very big potential safety hazard and environmental disaster to production, and gaseous The phosgene reaction cannot be completely quantified, the reaction conditions are harsh, the requirements for the reaction equipment are high, and the product yield and product quality are relatively low. (3) Contents of the invention [0003] The purpose of the present invention is to provide a simple and reasonable process, high safety, effective utilization of by-products, high reaction yield, high product purity, low production cost, and ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D223/22
Inventor 苏为科李坚军孙艳
Owner ZHEJIANG UNIV OF TECH
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