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    • 43. 发明授权
    • 하프늄 착체의 제조방법
    • 하프늄체체의제조방법
    • KR100932586B1
    • 2009-12-17
    • KR1020080060267
    • 2008-06-25
    • 샌트랄 글래스 컴퍼니 리미티드
    • 야마다슈헤이료카와아쯔시
    • C07F7/00
    • C07C49/92C07C29/70C07C41/18C07C45/77C07C31/28C07C43/04
    • 본 발명은 반도체 제조에 있어서의 성막(成膜)원료로서 적합한 테트라-t-부톡시하프늄[Hf(C
      4 H
      9 O)
      4 ], 테트라키스(아세틸아세토나토)하프늄[Hf(C
      5 H
      7 O
      2 )
      4 ], 테트라키스(1-메톡시-2-메틸-2-프로판올라토)하프늄[Hf(C
      5 H
      11 O
      2 )
      4 ], 테트라-t-아밀옥시하프늄[Hf(C
      5 H
      11 O)
      4 ], 테트라키스(3-메틸-3-펜톡시)하프늄[Hf(C
      6 H
      13 O)
      4 ], 및 테트라키스(헥사플루오로아세틸아세토나토)하프늄[Hf(C
      5 F
      6 HO
      2 )
      4 ]의 제조방법을 제공하는 것을 과제로 한다.
      본 발명은 상기 과제를 해결하기 위해, 테트라-t-부톡시하프늄, 테트라키스(아세틸아세토나토)하프늄, 테트라키스(1-메톡시-2-메틸-2-프로판올라토)하프늄, 테트라-t-아밀옥시하프늄, 테트라키스(3-메틸-3-펜톡시)하프늄, 및 테트라키스(헥사플루오로아세틸아세토나토)하프늄의 제조방법에 있어서, 화학식 Hf[N(R
      1 )(R
      2 )]
      4 로 표시되는 하프늄아미드 착체에 화학식 A(O
      y XO
      n R
      f )
      m 으로 표시되는 카르보닐기 또는 설포닐기를 함유하는 화합물을 첨가한 후, 감압증류를 행하는 공정(제1 공정), 제1 공정에 의해 얻어지는 유분(留分)에 화학식 Li(NR
      3 R
      4 )로 표시되는 리튬알킬아미드를 첨가한 후, 감압증류를 행하는 공정(제2 공정), 제2 공정에 의해 얻어지는 유분에 t-부탄올, 아세틸아세톤, 1-메톡시-2-메틸-2-프로판올, t-아밀알코올, 3-메틸-3-펜탄올, 또는 헥사플루오로아세틸아세톤 중 어느 하나를 첨가한 후, 감압증류를 행하 는 공정(제3 공정)을 순차 실시한다.
    • 公开了分别生产四叔丁醇铪,四(乙酰丙酮)铪,四(1-甲氧基-2-甲基-2-丙醇)铪,四叔戊醇铪,四(3-甲基 -3-戊氧基)铪和四(六氟乙酰丙酮)铪。 第一种方法包括以下步骤:(a)向粗铪酰胺Hf [N(R 1)(R 2)] 4中加入化合物A(O y XO n R f)m(例如CF 3 SO 3 H) (b)将步骤(a)的产物在减压下进行蒸馏; (c)将烷基酰胺锂Li(NR 3 R 4)加入由步骤(b)获得的馏分中; (d)将步骤(c)的产物在减压下进行蒸馏; (e)将叔丁醇加入步骤(d)获得的馏分中; 和(f)将步骤(e)的产物在减压下进行蒸馏。 步骤(e)的叔丁醇分别在第二至第六步中用乙酰丙酮,1-甲氧基-2-甲基-2-丙醇,叔戊醇,3-甲基-3-戊醇和六氟乙酰丙酮代替。
    • 48. 发明公开
    • 유기 불소화합물의 제조방법
    • 制备有机氟化合物的方法
    • KR1020030074946A
    • 2003-09-22
    • KR1020020013947
    • 2002-03-14
    • 주식회사 씨트리
    • 지대윤김동욱
    • C07D233/58
    • C07C17/208C07B39/00C07C41/18C07C41/22C07C45/63C07C43/225C07C43/215
    • PURPOSE: A process for preparing organic fluorine compounds is provided, thereby rapidly preparing the organic fluorine compounds in higher yield under mild condition. CONSTITUTION: A process for preparing organic fluorine compounds comprises the steps of: reacting alkyl halide or alkyl sulfonate with fluoride using imidazolium salt of formula 1 as a sole solvent or with organic solvent as mixed solvents, wherein R1 is C1-C18 alkyl; R2, R3, R4 and R5 are hydrogen or C1-C18 alkyl; n is an integer of 1 to 3; and A is anion capable of forming salt, wherein the anion is anion of MFk-, R6O-, R7R8N- or R9R10R11C-; M is an element from the periodic table, groups 3 to 15; k is an integer of 2 to 6; R6 is C1-C12 alkylsulfone, halo C1-C12 alkylsulfone, C1-C4 alkyl arylsulfone, halo arylsulfone, halosulfone, phosphoryl or perfluoro C1-C12 alkylcarbon; R7, R8, R9, R10 and R11 are independently C1-C12 alkylsulfone, halo C1-C12 alkylsulfone, C1-C4 alkyl arylsulfone and halo arylsulfone.
    • 目的:提供一种制备有机氟化合物的方法,从而在温和条件下以更高的产率快速制备有机氟化合物。 构成:制备有机氟化合物的方法包括以下步骤:使烷基卤化物或烷基磺酸盐与氟化物反应,使用式1的咪唑鎓盐作为单一溶剂或作为混合溶剂的有机溶剂,其中R 1为C 1 -C 18烷基; R2,R3,R4和R5是氢或C1-C18烷基; n为1〜3的整数, 并且A是能形成盐的阴离子,其中阴离子是MFk-,R6O-,R7R8N-或R9R10R11C-的阴离子; M是元素周期表中的元素,3〜15族; k为2〜6的整数, R6是C1-C12烷基砜,卤代C1-C12烷基砜,C1-C4烷基芳基砜,卤代芳基砜,卤代砜,磷酰基或全氟C1-C12烷基碳; R 7,R 8,R 9,R 10和R 11独立地为C 1 -C 12烷基砜,卤代C 1 -C 12烷基砜,C 1 -C 4烷基芳基砜和卤代芳基砜。
    • 49. 发明公开
    • 디알콕시부텐으로부터테트라히드로푸란의제조방법
    • 制备四氢呋喃的方法来自DIALKOXYBUTENES
    • KR1020000016343A
    • 2000-03-25
    • KR1019980709916
    • 1997-05-28
    • 바스프 에스이
    • 피숴,롤프핀코스,롤프쉐퍼,마르틴횐,아르투르쉬바브,페터
    • C07D307/08
    • C07C41/18C07C41/26C07C41/32C07D307/08C07C43/15C07C43/13
    • PURPOSE: A preparation method of tetrahydrofuran by reacting 1,4-butene diol dieter with water and hydrogen in the presence of catalysts or catalyst combinations is provided which can reduce the number of reaction step. CONSTITUTION: Tetrahydrofuran is prepared by reacting 1,4-butene diol dieter of formulae (I) RO-CH2-CH=CH-CH2-OR and/or (II) RO-CH2-CH2-CH=CH-OR, in which the R groups can be identical or different and stand for C1-15 alkyl or cycloalkyl groups, C6-12 aryl groups or C7-15 aralkyl groups, with water and hydrogen at temperatures of between 20 and 300°C and a pressure of between 1 and 300 bar in the presence of catalysts or catalyst combinations which both contain components which can hydrogenate and comprise acid or basic centers. The invention further concerns a novel process for preparing the 1,4-butene diol dieter of formula (I) by metathesis.
    • 目的:提供在催化剂或催化剂组合的存在下使1,4-丁二醇二酯与水和氢反应的四氢呋喃的制备方法,其可以减少反应步骤的数量。 构成:通过使式(I)RO-CH 2 -CH = CH-CH 2 -OR和/或(II)RO-CH 2 -CH 2 -CH = CH-OR的1,4-丁二醇二元酸酯反应制备四氢呋喃,其中 R基团可以相同或不同,代表C1-15烷基或环烷基,C6-12芳基或C7-15芳烷基,与水和氢在20〜300℃之间,压力为1 和300巴,在催化剂或催化剂组合的存在下,它们都含有可氢化并包含酸或碱性中心的组分。 本发明还涉及通过复分解制备式(I)的1,4-丁二醇二元醇的新方法。