KR960014150A - 결정형 수크랄로즈-6-에스테르의 중간 분리 없는 수크랄로즈의 제조방법 - Google Patents

결정형 수크랄로즈-6-에스테르의 중간 분리 없는 수크랄로즈의 제조방법 Download PDF

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KR960014150A
KR960014150A KR1019950035395A KR19950035395A KR960014150A KR 960014150 A KR960014150 A KR 960014150A KR 1019950035395 A KR1019950035395 A KR 1019950035395A KR 19950035395 A KR19950035395 A KR 19950035395A KR 960014150 A KR960014150 A KR 960014150A
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trichloro
iii
sucralose
product
acyl
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KR1019950035395A
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엘. 나비아 주안
이. 워크업 로버트
에스. 네이디치 데이빗
엠. 버논 니콜라스
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안드레아 엘.콜비
맥네일-피피씨, 인코포레이티드
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
    • C07H3/04—Disaccharides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
    • C07H5/02—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to halogen

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  • Organic Chemistry (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Saccharide Compounds (AREA)
  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Steroid Compounds (AREA)
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Abstract

본 발명은 중화된염소화 반응 혼합무로 부터 제3급 아미드 반응 부형물을 제거하기 전 또는 후에 바로 스크랄로즈-6-에스테르를 탈아실화함으로써 수크랄로즈 수용액 이외에 염과 불순물을 제조하고, 여기에서 추출에 의해 수크랄로즈를 회수하고, 바람직하게는 결정화에 의해 정제하는, 스크랄로즈-6-에스테르로 부터 수크랄로즈를 제조하는방법에 관한 것이다.

Description

결정형 스크랄로즈-6-에스테르의 중간 분리 없는 스크랄로즈의 제조방법
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (15)

  1. (i)3급 아미드를 함유하는 반응 매질에서 탈아실화르 수행하기에 충분한 온도 및 시간동안 (a) 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈, (b)알킬리 금속 또는 알칼리 토금속 염화물을 함유하는 염, (c)물, 및 (d)기타 염소화 수크로오즈 부산물의 수용액의 pH를 약 11(± 1)로 상승시킴으로써 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈를 탈아실화하여 수크랄 로즈, 알칼리 금속 또는 알칼리 토금속 염화물을 함유하는 염, 및 기타 염소화 수크로오즈 부산물을 함유하는 수용액을 생성시키고; (ii)3급 아미드를 제거하고; 및 (iii)상기 단계 (ii)의 생성물로 부터 스크랄로즈를 회수함을 특징으로 하여, 3급 아미드를 함유하는 반응 매질에서, 상기 (a), (b), (c) 및 (d)의 공급 혼합물로 부터 수크랄로즈를 제조하는 방법.
  2. 제1항에 있어서, 단계(ii)를 증기 스트립핑(stripping)에 의해 진행함을 특징으로 하는 방법.
  3. 제2항에 있엇, 3급 아미드가 N-N-디메틸포름아미드임을 특징으로 하는 방법.
  4. 제3항에 있어서, 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈가 6-O-아세틸-4, 1′, 6′-트리클로로-4, 1′, 6′-트리데옥시갈락토수크로오즈 또는 6-O-벤조일-4, 1′, 6′-트리클로로-4, 1′, 6′-트리데옥시갈락토수크로오즈임을 특징으로 하는 방법.
  5. 제4항에 있어서, 단계(iii)의 생성물로 부터 스크랄로즈를 추출하는 단계를 회분, 연속, 또는 연속 역류 추출에 의해 수행함을 특징으로 하는 방법.
  6. 제5항에 있어서, 수크랄로즈를 추가로 결정화에 의해 정제함으로 특징으로 하는 방법.
  7. 제6항에 있어서, 결정화를 물 또는 에틸아세테이트로 부터 수행함을 특징으로 하는 방법.
  8. (i)3급 아미드의 대부분을 제거하여 (a) 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈, (b)알킬리 금속 또는 알칼리 토금속 염화물을 함유하는 염 및 (d)기타 염소화 수크로오즈 부산물의 수용액을 제조하고; (ii)탈아실화를 수행하기에 충분한 온도 및 시간동안 상기 단계(i)의 수용액 생성물의 pH를 약 11(± 1)로 상승시킴으로써 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈를 탈아실화하여 수크랄 로즈, 알칼리 금속 또는 알칼리 토금속 염화물을 함유하는 염, 및 기타 염소화 수크로오즈 부산물을 함유하는 수용액을 생성시키고; 및 (iii)상기 단계 (ii)의 생성물로 부터 스크랄로즈를 회수함을 특징으로 하여, 3급 아미드를 함유하는 반응 매질에서, 상기 (a), (b), (c) 및 (d)의 공급 혼합물로 부터 수크랄로즈를 제조하는 방법.
  9. 제8항에 있어서, 6-O-아실-4, 4′, 6′ -트리클로로-4, 1′, 6′ -트리데옥시-갈락토수크로오즈가 6-O-아세틸-4, 1′, 6′-트리클로로-4, 1′, 6′-트리데옥시갈락토수크로오즈 또는 6-O-벤조일-4, 1′, 6′-트리클로로-4, 1′, 6′-트리데옥시갈락토수크로오즈임을 특징으로 하는 방법.
  10. 제9항에 있어서, 단계(iii)은 유기 용매에 의해 단계(ii)의 생성물로 부터 스크랄로즈를 추출한 후, 이 유기 용매로부터 스크랄로즈르 결정화시킴으로써 수행함을 특징으로 하는 방법.
  11. 제10항에 있어서, 유기 용매가 에틸렌아세테이트임을 특징으로 하는 방법.
  12. 제9항에 있어서, 단계(iii)은 유기 용매에 의해 단계(ii)의 생성물로 부터 스크랄로즈를 추출한 후, 물로부터 수크랄로즈를 결정화시킴으로써 수행함을 특징으로 하는 방법.
  13. 제9항에 있어서, 3급 아미드가 N,N-디메틸포름아미드임을 특징으로 하는 방법.
  14. 제13항에 있어서, 단계(i)에서 3급 아미드의 제거를 수증기 증류에 의해 수행함을 특징으로 하는 방법.
  15. 제11항에 있어서, 단계(ii)의 생성물로 수크랄로즈를 추출하는 단계를 회분, 연속, 또는 역류 추출에 의해 수행함을 특징으로 하는 방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950035395A 1994-10-17 1995-10-13 결정형수크랄로즈-6-에스테르의중간분리없는수크랄로즈의제조방법 KR100390629B1 (ko)

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US32395494A 1994-10-17 1994-10-17
US08/323954 1994-10-17
US08/448710 1995-05-24
US08/448,710 US5498709A (en) 1994-10-17 1995-05-24 Production of sucralose without intermediate isolation of crystalline sucralose-6-ester

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AU (1) AU707557B2 (ko)
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