KR960007542A - Method for preparing 4-chloro-2,5-dialkoxy aniline and purification method thereof - Google Patents

Method for preparing 4-chloro-2,5-dialkoxy aniline and purification method thereof Download PDF

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Publication number
KR960007542A
KR960007542A KR1019940020113A KR19940020113A KR960007542A KR 960007542 A KR960007542 A KR 960007542A KR 1019940020113 A KR1019940020113 A KR 1019940020113A KR 19940020113 A KR19940020113 A KR 19940020113A KR 960007542 A KR960007542 A KR 960007542A
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South Korea
Prior art keywords
chloro
dialkoxy
nitrobenzene
aniline
solvent
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KR1019940020113A
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Korean (ko)
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KR100332212B1 (en
Inventor
이정민
고재천
김범식
정순용
서정권
심호섭
주정표
장유식
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강박광
재단법인 한국화학연구소
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Priority to KR1019940020113A priority Critical patent/KR100332212B1/en
Publication of KR960007542A publication Critical patent/KR960007542A/en
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Publication of KR100332212B1 publication Critical patent/KR100332212B1/en

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
    • C07C217/78—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having amino groups and etherified hydroxy groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

본 발명은 4-클로로-2,5-디알콕시 니트로벤젠을 아세토 니트릴 또는 그의 수용액을 용매로 하여 촉매의 황화처리 여부에 관계없이 백금계 담지 촉매하에 수소환원시켜 탈염소화 없이 4-클로로-2,5-디알콕시 아닐린을 제조하는 방법에 관한 것이며 또한 생성 혼합물을 산석(酸析) 또는 염석(鹽析)을 통해 정제함으로써 반응물의 순도에 관계없이 고순도의 4-클로로-2,5-디알콕시 아닐린을 얻는 정제 방법에 관한 것이다.The present invention provides 4-chloro-2,5-dialkoxy nitrobenzene as a solvent using acetonitrile or its aqueous solution as a solvent and hydrogen reduction under a supported catalyst based on platinum, regardless of whether the catalyst is sulfided. It relates to a process for preparing 5-dialkoxy aniline and also to purifying the resulting mixture through calcination or salting-out of high purity 4-chloro-2,5-dialkoxy aniline regardless of the purity of the reactants. It relates to a purification method to obtain.

Description

4-클로로-2,5-디알콕시 아닐린의 제조방법 및 그 정제법Method for preparing 4-chloro-2,5-dialkoxy aniline and its purification

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (7)

4-클로로-2,5-디알콕시 니트로벤젠을 용매로서 아세토니트릴 또는 그의 수용액을 사용하여 촉매 수소환원시켜 4-클로로-2,5-디알콕시 아닐린을 제조하는 방법.A process for producing 4-chloro-2,5-dialkoxy aniline by catalytic hydrogen reduction of 4-chloro-2,5-dialkoxy nitrobenzene as a solvent using acetonitrile or an aqueous solution thereof. 제1항에 있어서, 촉매로는 일반 백금 담지 촉매 또는 변형된 백금 담지 촉매를 사용하는 것을 특징으로 하는 방법.The method according to claim 1, wherein the catalyst is a conventional platinum supported catalyst or a modified platinum supported catalyst. 제1항에 있어서, 수소 20-180psi 가압하, 20-80℃의 온도에서 행해지는 것을 특징으로 하는 방법.The method of claim 1 wherein the hydrogen is carried out at a temperature of 20-80 ° C. under 20-180 psi pressurization. 제1항 내지 제3항중의 어느 한 항에 있어서, 반응 완료후 증류 또는 공비증류하여 회수한 용매를 재사용하는 것을 특징으로 하는 방법.The method according to any one of claims 1 to 3, wherein the solvent recovered by distillation or azeotropic distillation after the completion of the reaction is reused. 제1항 내지 제4항중의 어느 한 항에 있어서, 4-클로로-2,5-디알콕시 니트로벤젠은 4-클로로-2,5-디메녹시 니트로벤젠 또는 4-클로로-2,5-디에콕시 니트로벤젠인 것을 특징으로 하는 방법.The 4-chloro-2,5-dialkoxy nitrobenzene according to any one of claims 1 to 4 is 4-chloro-2,5-dimenoxy nitrobenzene or 4-chloro-2,5-diene. It is a cocci nitrobenzene. 4-클로로-2,5-디알콕시 니트로벤젠을 용매로서 아세토니트릴 또는 그의 수용액을 사용하여 촉매 수소환원시켜 제조된 4-클로로-2,5-디알콕시 아닐린을 염화수소가스 또는 염산 수용액과 알칼리를 사용하여 염석 또는 산석하는 것을 특징으로 하는 4-클로로-2,5-디알콕시 아닐린의 정제법.4-chloro-2,5-dialkoxy nitrobenzene was prepared by catalytic hydrogen reduction using acetonitrile or its aqueous solution as a solvent, and 4-chloro-2,5-dialkoxy aniline was prepared using hydrogen chloride gas or aqueous hydrochloric acid solution and alkali. Purification of 4-chloro-2,5-dialkoxy aniline, characterized in that the salt is formed or acidified. 제6항에 있어서, 알칼리로는 NaOH를 사용하는 것을 특징으로 하는 방법.7. The method of claim 6, wherein NaOH is used as the alkali. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019940020113A 1994-08-14 1994-08-14 Process for producing 4-chloro-2,5-dialkoxy aniline and refining method thereof KR100332212B1 (en)

Priority Applications (1)

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KR1019940020113A KR100332212B1 (en) 1994-08-14 1994-08-14 Process for producing 4-chloro-2,5-dialkoxy aniline and refining method thereof

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Application Number Priority Date Filing Date Title
KR1019940020113A KR100332212B1 (en) 1994-08-14 1994-08-14 Process for producing 4-chloro-2,5-dialkoxy aniline and refining method thereof

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KR960007542A true KR960007542A (en) 1996-03-22
KR100332212B1 KR100332212B1 (en) 2002-11-14

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US41671A (en) * 1864-02-23 Henry bennett
DE2521303B2 (en) * 1975-05-13 1977-09-22 Bayer Ag, 5090 Leverkusen PROCESS FOR THE PREPARATION OF 2,5-DIMETHOXY-4-CHLORANILINE

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