KR930023330A - Method for preparing 3-amino-4-methoxyacetanilide - Google Patents

Method for preparing 3-amino-4-methoxyacetanilide Download PDF

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KR930023330A
KR930023330A KR1019920008170A KR920008170A KR930023330A KR 930023330 A KR930023330 A KR 930023330A KR 1019920008170 A KR1019920008170 A KR 1019920008170A KR 920008170 A KR920008170 A KR 920008170A KR 930023330 A KR930023330 A KR 930023330A
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South Korea
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amino
represented
methoxyacetanilide
producing
reaction
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KR1019920008170A
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Korean (ko)
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KR950002836B1 (en
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송현삼
김종범
조정학
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오재덕
한국화약 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C235/00—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by oxygen atoms
    • C07C235/42—Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by oxygen atoms having carbon atoms of carboxamide groups bound to carbon atoms of six-membered aromatic rings and singly-bound oxygen atoms bound to the same carbon skeleton

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

Abstract

본 발명은 하기 구조식(Ⅰ)로 표시되는 3-아미노-4-메톡시아세트아닐리드의 제조방법에 관한 것으로, 좀더 구체적으로는 알콜용매하에서 하기 구조식(Ⅱ)로 표시되는 2,4-디아미노아니솔를 하기 구조식(Ⅲ)으로 표시되는 아세트산 무수물을 아세틸화 반응시켜 하기 구조식(Ⅰ)로 표시되는 3-아미노-4-메톡시아세트아닐리드를 고수율 및 고순도로 제조하는 방법에 관한 것이다.The present invention relates to a method for preparing 3-amino-4-methoxyacetanilide represented by the following structural formula (I), more specifically 2,4-diaminoani represented by the following structural formula (II) under an alcohol solvent. It relates to a method for producing 3-amino-4-methoxyacetanilide represented by the following structural formula (I) by acetylating an acetic anhydride represented by the following structural formula (III) to a high yield and high purity.

Description

3-아미노-4메톡시아세트아닐리드의 제조방법Method for preparing 3-amino-4methoxyacetanilide

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

Claims (7)

하기 구조식(Ⅰ)의 제조방법에 있어서, 알콜용매하에서 하기 구조식(Ⅲ)을 pH가 8~10.5의 범위에서 아세틸화 반응시켜 제조하는 것을 특징으로 하는 3-아미노-4-메톡시아세트아닐리드의 제조방법.In the production method of the following formula (I), 3-amino-4-methoxyacetanilide is prepared by acetylation of the following formula (III) in an alcohol solvent in a pH range of 8 to 10.5. Way. 제1항에 있어서, 상기 구조식(Ⅱ)로 표시되는 2,4-디아미노아니솔을 알콜용매하에서 상기 구조식(Ⅲ)으로 표시되는 아세트산 무수물과 8~10.5의 pH에서 아세틸화 반응시키고, 상기 구조식(Ⅰ)로 표시되는 3-아미노-4메톡시아세트아닐리드를 염산염으로 분리하고 난후 진한염산으로 반응여액에 함유된 2,4-디아세틸아미노아니솔을 2,4-디아미노아니솔로 가수분해시켜 회수하여 재사용하는 것을 특징으로 하는 3-아미노-4메톡시아세트아닐리드의 제조방법.The acetylating reaction of claim 1, wherein the 2,4-diaminoanisole represented by Structural Formula (II) is subjected to an acetylation reaction with an acetic anhydride represented by Structural Formula (III) under an alcohol solvent at a pH of 8 to 10.5. The 3-amino-4methoxyacetanilide represented by (I) was isolated with hydrochloride, and then hydrolyzed 2,4-diacetylaminoanisole contained in the reaction filtrate with concentrated hydrochloric acid to 2,4-diaminoanisole. A method for producing 3-amino-4methoxyacetanilide, which is recovered and reused. 제1항 또는 제2항에 있어서, 상기 반응물의 반응온도가 -5~10℃의 점위에서 반응하는 것을 특징으로 하는 3-아미노-4-메톡시아세트아닐리드의 제조방법.The method for producing 3-amino-4-methoxyacetanilide according to claim 1 or 2, wherein the reaction temperature of the reactants is reacted at a point of -5 to 10 ° C. 제1항 또는 제2항에 있어서, 상기 알콜용매의 탄소수가 1~4인 알콜을 반응하는 것을 특징으로 하는 3-아미노-4-메톡시아세트아닐리드의 제조방법.The method for producing 3-amino-4-methoxyacetanilide according to claim 1 or 2, wherein the alcohol having 1 to 4 carbon atoms is reacted. 제4항에 있어서, 상기 알콜용매가 메탄올 또는 에탄올임을 특징으로 하는 3-아미노-4-메톡시아세트아닐리드의 제조방법.The method of claim 4, wherein the alcohol solvent is methanol or ethanol. 제1항 또는 제2항에 있어서, 상기 pH의 범위가 수산화칼륨용액에 의해 유지됨을 특징으로 하는 3-아미노-4-메톡시아세트아닐리드의 제조방법.The process for producing 3-amino-4-methoxyacetanilide according to claim 1 or 2, wherein the pH range is maintained by a potassium hydroxide solution. 제1항 또는 제2항에 있어서, 상기 pH를 유지하기 위하여 반응시작시 또는 반응도중에 상기 구조식(Ⅱ)로 표시되는 2,4-디아미노아니솔 1몰에 대하여 하기 일반식(Ⅶ)로 표시되는 금속옥시드의 총투입량을 0.1 몰 내지 5.0몰 사용하고 상기 구조식(Ⅲ)으로 표시되는 아세트산 무수물을 분할주입하여 반응하는 것을 특징으로 하는 상기 구조식(Ⅰ)로 표시되는 3-아미노-4-메톡시아세트아닐리드의 제조방법.The method according to claim 1 or 2, wherein in order to maintain the pH, 1 mole of 2,4-diaminoanisole represented by the structural formula (II) at the beginning or during the reaction is represented by the following general formula (VII). 3-amino-4-meth represented by the above formula (I), wherein the total amount of the metal oxide to be used is 0.1 mol to 5.0 mol and the acetic anhydride represented by the above formula (III) Method for preparing oxyacetanilide. M(OH)n(Ⅶ)M (OH) n (Ⅶ) MmO (Ⅷ)MmO (Ⅷ) 상기 식에서, M은 알칼리금속 양이온(이때, n=1, m=2) 또는 알칼리 토금속양이온(이때 m=2, n=1)이다.Wherein M is an alkali metal cation (where n = 1, m = 2) or an alkaline earth metal cation (where m = 2, n = 1). ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019920008170A 1992-05-14 1992-05-14 Process for the preparation of 3-amino-4-methoxyacetanilide KR950002836B1 (en)

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KR1019920008170A KR950002836B1 (en) 1992-05-14 1992-05-14 Process for the preparation of 3-amino-4-methoxyacetanilide

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KR1019920008170A KR950002836B1 (en) 1992-05-14 1992-05-14 Process for the preparation of 3-amino-4-methoxyacetanilide

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KR930023330A true KR930023330A (en) 1993-12-18
KR950002836B1 KR950002836B1 (en) 1995-03-27

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