METHOD FOR PREPARING 3-CARBAMOYMETHYL-5-METHYLHEXANOIC ACID IN RECYCLING WAY

METHOD FOR PREPARING 3-CARBAMOYMETHYL-5-METHYLHEXANOIC ACID IN RECYCLING WAY

The present invention provides a method for recycling 3-carbamoymethyl-5-methylhexanoic acid from 3-carbamoymethyl-5-methylhexanoic acid chiral resolving mother liquor. The method comprises the following steps: (a) distilling 3-carbamoymethyl-5-methylhexanoic acid chiral resolving mother liquor, add...

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Hauptverfasser: Zhang Wenling, Wang Shudong, You Xuehai
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ACYCLIC OR CARBOCYCLIC COMPOUNDS
CHEMISTRY
COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM,RUBIDIUM, CAESIUM, OR FRANCIUM
INORGANIC CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
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creator Zhang Wenling
Wang Shudong
You Xuehai
description The present invention provides a method for recycling 3-carbamoymethyl-5-methylhexanoic acid from 3-carbamoymethyl-5-methylhexanoic acid chiral resolving mother liquor. The method comprises the following steps: (a) distilling 3-carbamoymethyl-5-methylhexanoic acid chiral resolving mother liquor, adding aromatic hydrocarbon, heating to dissolve, keeping the temperature and stirring; (b) after completing the reaction in step (a), cooling the reaction solution to 30-60° C., then adding alkali liquor dropwise, keeping the temperature and reacting; and (c) after completing the reaction in step (b), cooling the reactant to 20-30° C., layering, adjusting the pH of the separated water layer to 1 to 2, performing extraction by using an organic solvent, distilling an organic phase under a reduced pressure, and crystallizing at 0±5° C. to obtain 3-carbamoymethyl-5-methylhexanoic acid. The method provided in the present invention is convenient to operate, and the recycled product is high in purity (≧99.8%) and yield.
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The method comprises the following steps: (a) distilling 3-carbamoymethyl-5-methylhexanoic acid chiral resolving mother liquor, adding aromatic hydrocarbon, heating to dissolve, keeping the temperature and stirring; (b) after completing the reaction in step (a), cooling the reaction solution to 30-60° C., then adding alkali liquor dropwise, keeping the temperature and reacting; and (c) after completing the reaction in step (b), cooling the reactant to 20-30° C., layering, adjusting the pH of the separated water layer to 1 to 2, performing extraction by using an organic solvent, distilling an organic phase under a reduced pressure, and crystallizing at 0±5° C. to obtain 3-carbamoymethyl-5-methylhexanoic acid. 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subjects ACYCLIC OR CARBOCYCLIC COMPOUNDS
CHEMISTRY
COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM,RUBIDIUM, CAESIUM, OR FRANCIUM
INORGANIC CHEMISTRY
METALLURGY
ORGANIC CHEMISTRY
title METHOD FOR PREPARING 3-CARBAMOYMETHYL-5-METHYLHEXANOIC ACID IN RECYCLING WAY
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