KR970042537A - Method for selectively separating catechol from a mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol and catechol - Google Patents

Method for selectively separating catechol from a mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol and catechol Download PDF

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Publication number
KR970042537A
KR970042537A KR1019950065552A KR19950065552A KR970042537A KR 970042537 A KR970042537 A KR 970042537A KR 1019950065552 A KR1019950065552 A KR 1019950065552A KR 19950065552 A KR19950065552 A KR 19950065552A KR 970042537 A KR970042537 A KR 970042537A
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South Korea
Prior art keywords
catechol
mixture
dihydro
dimethyl
benzofuranol
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KR1019950065552A
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Korean (ko)
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KR100377447B1 (en
Inventor
이중환
박은정
이길성
Original Assignee
황선두
삼성종합화학 주식회사
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Priority to KR1019950065552A priority Critical patent/KR100377447B1/en
Publication of KR970042537A publication Critical patent/KR970042537A/en
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Publication of KR100377447B1 publication Critical patent/KR100377447B1/en

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
    • C07D307/79—Benzo [b] furans; Hydrogenated benzo [b] furans with only hydrogen atoms, hydrocarbon or substituted hydrocarbon radicals, directly attached to carbon atoms of the hetero ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01—Preparation of ethers
    • C07C41/34—Separation; Purification; Stabilisation; Use of additives
    • C07C41/44—Separation; Purification; Stabilisation; Use of additives by treatments giving rise to a chemical modification

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

Abstract

본 발명은 2,3-디히드로-2,2-디메틸-7-벤조푸란올(이하 "7-OH"라 한다)과 카테콜을 함유하는 혼합물로부터 카테콜을 선택적으로 제거하여 높은 순도의 7-OH를 얻는 방법에 관한 것이다. 기존에는 카테콜과 메타알릴클로라이드로부터 7-OH를 제조함에 있어, 반응 혼합물로부터 카테콜을 액체-액체 추출법을 이용하여 분리 회수하였으나, 이는 7-OH와 카테콜을 분리하는 직접적인 방법은 아니고, 추출효과를 높이기 위해 붕산 또는 붕사등의 붕소화합물을 첨가하여 추출하였으나 다량의 붕소화합물의 소비되며 다량의 폐수 발생으로 바람직하지 않다. 본 발명은 7-OH와 카테콜의 혼합물에서 무기염을 가하여 카테콜을 선택적으로 제거하여 고순도의 7-OH를 분리 회수하는 방법이다.The present invention provides high purity 7 by selectively removing catechol from a mixture containing 2,3-dihydro-2,2-dimethyl-7-benzofuranol (hereinafter referred to as "7-OH") and catechol. It relates to a method of obtaining -OH. Conventionally, in the preparation of 7-OH from catechol and methallyl chloride, catechol was separated and recovered from the reaction mixture by liquid-liquid extraction, but this was not a direct method of separating 7-OH and catechol. In order to enhance the effect, it is extracted by adding a boron compound such as boric acid or borax, but a large amount of boron compound is consumed and is not preferable due to the generation of a large amount of waste water. The present invention is a method for separating and recovering high purity 7-OH by selectively removing catechol by adding an inorganic salt in a mixture of 7-OH and catechol.

Description

2,3-디히드로-2,2-디메틸-7-벤조푸란올과 카테콜의 혼합물로부터 카테콜을 선택적으로 분리하는 방법Method for selectively separating catechol from a mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol and catechol

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

Claims (3)

카테콜과 2,3-디히드로-2,2-디메틸-7-벤조푸란올을 함유하는 혼합물로부터 이를 분리 회수하는 방법에 있어서, 상기 혼합물을 유기 용매에 녹이고 카테콜 1당량에 대하여 1-2당량의 무기염을 가한 후 50-150℃로 환류하여 케테콜-무기염 복합체의 침전물을 얻고 이 침전물을 여과 분리한 유기 용매 상으로부터 2,3-디히드로-2,2-디메틸-7-벤조푸란올을 분리 회수하고 상기의 카테콜-무기염 복합체에 20-50ml의 물을 가하여 상기 카테콜-무기염 복합체로부터 높은 순도로 카테콜과 무기염을 회수하는 방법A method for separating and recovering a catechol from a mixture containing 2,3-dihydro-2,2-dimethyl-7-benzofuranol, wherein the mixture is dissolved in an organic solvent and 1-2 equivalents of catechol is used. After addition of an equivalent amount of an inorganic salt, the mixture was refluxed at 50-150 ° C. to obtain a precipitate of the ketchol-inorganic salt complex, and the precipitate was filtered off from an organic solvent separated by 2,3-dihydro-2,2-dimethyl-7-benzo. Separation and recovery of furanol and 20-50ml of water to the catechol-inorganic salt complex to recover catechol and inorganic salts from the catechol-inorganic salt complex in high purity 제1항에 있어서, 무기염으로 MgCl2, MgBr2, mG(OEt)2, FeCl2를 사용하는 방법The method of claim 1, wherein MgCl 2 , MgBr 2 , mG (OEt) 2 , FeCl 2 are used as inorganic salts. 제1항에 있어서, 용매로 MIBK, 톨루엔을 사용하는 방법The method of claim 1, wherein MIBK and toluene are used as a solvent.
KR1019950065552A 1995-12-29 1995-12-29 Process for selectively removing catechol from mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol(7-oh) and catechol KR100377447B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019950065552A KR100377447B1 (en) 1995-12-29 1995-12-29 Process for selectively removing catechol from mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol(7-oh) and catechol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019950065552A KR100377447B1 (en) 1995-12-29 1995-12-29 Process for selectively removing catechol from mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol(7-oh) and catechol

Publications (2)

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KR970042537A true KR970042537A (en) 1997-07-24
KR100377447B1 KR100377447B1 (en) 2003-06-09

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KR1019950065552A KR100377447B1 (en) 1995-12-29 1995-12-29 Process for selectively removing catechol from mixture of 2,3-dihydro-2,2-dimethyl-7-benzofuranol(7-oh) and catechol

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Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4420642A (en) * 1982-02-18 1983-12-13 Fmc Corporation Selective removal and recovery of catechol mixed with 2-methallyloxyphenol
JPH0699350B2 (en) * 1986-01-14 1994-12-07 三菱化成株式会社 Method for separating phenols and catechols
JPH05219966A (en) * 1992-02-12 1993-08-31 Showa Denko Kk Production of catechol
JP2557598B2 (en) * 1992-08-19 1996-11-27 三菱化学株式会社 Manufacturing method of catechols

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