SEPARATION OF METHOXYAZONITRILE

SEPARATION OF METHOXYAZONITRILE

PURPOSE:To prepare the titled compound useful as a polymerization catalyst, in high quality and yield, by reacting 2,2'-hydrazo-bis(4-methoxy-2,4-dimethylvalero- nitrile) with a halogen at a specific low temperature, and separating the objective compound at a specific temperature. CONSTITUTION:...

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Hauptverfasser: NAGAOKA JIYOUJI, NAWA HIROMI, YAMASHITA KAZUHIKO
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ACYCLIC OR CARBOCYCLIC COMPOUNDS
CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
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creator NAGAOKA JIYOUJI
NAWA HIROMI
YAMASHITA KAZUHIKO
description PURPOSE:To prepare the titled compound useful as a polymerization catalyst, in high quality and yield, by reacting 2,2'-hydrazo-bis(4-methoxy-2,4-dimethylvalero- nitrile) with a halogen at a specific low temperature, and separating the objective compound at a specific temperature. CONSTITUTION:2,2'-Hydrazo-bis(4-methoxy-2,4-dimethylvaleronitrile) of formulaI is made to react with the halogen of formula X2 (e.g. Cl, Br, etc.) at -60- -11 deg.C, and the crystals precipitated from the reaction liquid are separated at
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CONSTITUTION:2,2'-Hydrazo-bis(4-methoxy-2,4-dimethylvaleronitrile) of formulaI is made to react with the halogen of formula X2 (e.g. Cl, Br, etc.) at -60- -11 deg.C, and the crystals precipitated from the reaction liquid are separated at &lt;=-20 deg.C to obtain the objective compound of formula II. The reaction is carried out in a solvent such as methanol, isopropanol, etc., and the amount of the halogen is equivalent or somewhat excess to the compound of formulaI. The reaction system is cooled by circulating a cooling medium such as an aqueous solution of calcium chloride cooled with e.g. a two-stage compression refrigerator. 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CONSTITUTION:2,2'-Hydrazo-bis(4-methoxy-2,4-dimethylvaleronitrile) of formulaI is made to react with the halogen of formula X2 (e.g. Cl, Br, etc.) at -60- -11 deg.C, and the crystals precipitated from the reaction liquid are separated at &lt;=-20 deg.C to obtain the objective compound of formula II. The reaction is carried out in a solvent such as methanol, isopropanol, etc., and the amount of the halogen is equivalent or somewhat excess to the compound of formulaI. The reaction system is cooled by circulating a cooling medium such as an aqueous solution of calcium chloride cooled with e.g. a two-stage compression refrigerator. 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CONSTITUTION:2,2'-Hydrazo-bis(4-methoxy-2,4-dimethylvaleronitrile) of formulaI is made to react with the halogen of formula X2 (e.g. Cl, Br, etc.) at -60- -11 deg.C, and the crystals precipitated from the reaction liquid are separated at &lt;=-20 deg.C to obtain the objective compound of formula II. The reaction is carried out in a solvent such as methanol, isopropanol, etc., and the amount of the halogen is equivalent or somewhat excess to the compound of formulaI. The reaction system is cooled by circulating a cooling medium such as an aqueous solution of calcium chloride cooled with e.g. a two-stage compression refrigerator. The objective compound having light color and low irritant smell can be obtained by this reaction process.</abstract><oa>free_for_read</oa></addata></record>
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subjects ACYCLIC OR CARBOCYCLIC COMPOUNDS
CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
title SEPARATION OF METHOXYAZONITRILE
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