• 제목/요약/키워드: Tributylamine

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팔라듐 촉매를 이용한 디비닐케톤과 디비닐 ${\alpha}$-디케톤의 새로운 합성 (Palladium Catalyzed New Synthesis of Divinyl Ketones and Divinyl ${\alpha}$-Diketones)

  • 김진일;이광혁;임승재
    • 대한화학회지
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    • 제33권5호
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    • pp.522-529
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    • 1989
  • 팔라듐 촉매를 이용하여 할로겐화 비닐의 CO 첨가반응과 짝지음 반응을 동시에 진행시키는 CO 첨가 호모 짝지음 반응을 실시하여 비교적 좋은 수득률로 대칭 디비닐케톤 및 디비닐 ${\alpha}$-디케톤을 합성하였다. 촉매로는 palladium(II) acetate에 2mol%의 리간드를 사용하고 염기는 3당량의 tributylamine, 극성 용매를 사용하여 10기압의 일산화탄소 존재 하에 $100^{\circ}C$에서 반응을 실시한 경우 디비닐 ${\alpha}$-디케톤을 가장 좋은 수득률로 얻을 수 있었으며, 일산화탄소 상압 하에서는 주로 디비닐케톤이 합성되었다. 또한, 여러가지 할로겐화 비닐에 대해 위와 같은 반응조건으로 반응을 실시해 본 결과 예상한 대로 순조롭게 반응이 진행되어 여러가지의 디비닐케톤 및 디비닐 ${\alpha}$-디케톤을 선택적으로 합성할 수 있음을 확인하였다.

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Development of an Isolable Active Ester, Diethyl Thiophosphoryl [(Z)-(2-Aminothiazol-4-yl)-2-(Methoxyimino)acetate (DAMA) for the Synthesis of Cefotaxime

  • Yoon, Man-Young;Lee, Hee-Bong;Shin, Hyun-Ik
    • Bulletin of the Korean Chemical Society
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    • 제32권2호
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    • pp.407-410
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    • 2011
  • An isolable activated ester, diethyl thiophosphoryl [(Z)-(2-aminothiazol-4-yl)-2-(methoxyimino)acetate (9a, DAMA) was prepared in high purity, which was at least stable for 7 d at $25^{\circ}C$ and 6 months at $5^{\circ}C$. Its reaction with 7-ACA (4) in the presence of tributylamine in i-PrOH provided cefotaxime (1) of high purity in good yield. Preparation of DAMA and its reaction with 7-ACA (4) to 1 was performed in one-pot manner, respectively with minimal unit operations of stirring and filtration.

Syntheses and Thermal Properties of 5,10-Disubstituted-2,3,7,8-tetracyano-5,10-dihydrodipyrazino [2,3-b:2′,3′-el pyrazines and Polymeric Porphyrazines Derived from 2,3-Dichloro-5,6-dicyanopyrazine

  • Jaung, Jae-yun;Kim, Sung-Dong
    • Fibers and Polymers
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    • 제1권2호
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    • pp.71-75
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    • 2000
  • Intermolecular cyclization of 2-alkylamino-3-chloro-5,6-dicyanopyrazine 2 in the presence of tributylamine in N,N-dimethylformamide (DMF) gave 5,10-disubstituted-2,3,7,8-tetracyano -5,10-dihydrodipyrazino〔2,3-b:2',3'-e]pyrazines 3, which showed strong mesomorphic property and were anticipated as new chromophoric system for functional dye materials. Absorption spectra, fluorescent properties and other physical properties were correlated with their chemical structures. Vanadyl oligomeric porphyrazine with long alkyl groups synthesized from 3 had satisfactory solubility in tetrahydrofuran (THF), diethyl ether and dimethylsulfoxide (DMSO). The syntheses and characterization of vanadyl polymeric porphyrazines derived from 3 with long alkyl groups are reported.

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