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  • Reactions of Vinylogous Amides Tethered with a, b-Unsaturated Iminiums. A Formal Total Synthesis of (+)-Gephyrotoxin
    2015
    Co-Authors: Lin-li Wei, Richard P. Hsung, Heather M. Sklenicka, Aleksey I. Gerasyuto, Tbscl Imid
    Abstract:

    To a round bottom flask is added 0.178 mol propargyl alcohol, and 350 mL THF. The reaction is cooled to 0 oC followed by addition of 0.196 mol TBSCl, 0.2 mol imidazole, and 0.017 mol DMAP. The reaction is stirred and allowed to come to room temperature. Upon completion by TLC the solvent is removed and column chromatography gave 91 % yield of the protected alcohol. The protected alcohol (80.7 mmol) was dissolved in 225 mL THF and HMPA (1.44 mL) as well as 3 mg triphenylmethanol were added. This solution was cooled to –40 oC (dry ice/acetone) and 80.7 mmol n-BuLi (2.18 M in hexanes) is added dropwise. After stirring for 30 minutes the reaction is warmed to room temperature. 1,3-dibromopropane (for hexenol) or 1,4-dibromobutane (for heptenol) (161.4 mmol) is then filtered through silica and added to the reaction mixture. The reaction was allowed to stir for 2 days at room temperature. Quenching of the reaction was done with dropwise addition of water. THF was removed under reduced pressure, and extracted from ether/water. Removal of solvents from the organic layer followed by distillation of the excess dibromopropane gave 53 % yield of the alkyne. The alkyne is then dissolved in 45 mL DMSO and to that is added 0.0639 mol sodium azide. The reaction is placed under nitrogen and allowed to stir at room temperature for 18 hours. An equal volume of water was then added followed by extraction with ether, washing of the organic layer with brine, and drying over sodium sulfate. Solvent was removed from the organic layer and flash column chromatography was used to further purify the compound. The azide (6.4 mmol) was then dissolved in 20 mL THF. This solution was transferred by cannula to 60 mL THF containing 57.6 mmol lithium aluminum hydride. Refluxing of the solution continued for 20 hours. The reaction mixture was cooled to 0 oC and saturated sodium sulfate was slowly added unti

  • A Novel and Highly Stereoselective Intramolecular Formal [3+3] Cycloaddition Reaction of Vinylogous Amides Tethered with α,β-Unsaturated Aldehydes: A Formal Total Synthesis of (+)-Gephyrotoxin.
    Angewandte Chemie (International ed. in English), 2001
    Co-Authors: Lin-li Wei, Richard P. Hsung, Heather M. Sklenicka, Aleksey I. Gerasyuto
    Abstract:

    Complex piperidinyl heterocycles (for example, 2) were accessed by using a novel intramolecular formal [3+3] cycloaddition reaction of vinylogous amides tethered with enals (for example, 1). This method has been applied to a formal total synthesis of (+)-Gephyrotoxin (3).

  • Highly Stereoselective Intramolecular Formal (3 + 3) Cycloaddition Reactions of Vinylogous Amides Tethered with α , β β -Unsaturated Iminiums. A Formal Total Synthesis of (+)-Gephyrotoxin
    2001
    Co-Authors: Lin-li Wei, Heather M. Sklenicka, Aleksey I. Gerasyuto, Richard P. Hsung
    Abstract:

    To a round bottom flask is added 0.178 mol propargyl alcohol, and 350 mL THF. The reaction is cooled to 0 C followed by addition of 0.196 mol TBSCl, 0.2 mol imidazole, and 0.017 mol DMAP. The reaction is stirred and allowed to come to room temperature. Upon completion by TLC the solvent is removed and column chromatography gave 91% yield of the protected alcohol. The protected alcohol (80.7 mmol) was dissolved in 225 mL THF and HMPA (1.44 mL) as well as 3 mg triphenylmethanol were added. This solution was cooled to –40 C (dry ice/acetone) and 80.7 mmol n-BuLi (2.18 M in hexanes) is added dropwise. After stirring for 30 minutes the reaction is warmed to room temperature. 1,3-dibromopropane (for hexenol) or 1,4dibromobutane (for heptenol) (161.4 mmol) is then filtered through silica and added to the reaction mixture. The reaction was allowed to stir for 2 days at room temperature. Quenching of the reaction was done with dropwise addition of water. THF was removed under reduced pressure, and extracted from ether/water. Removal of solvents from the organic layer followed by distillation of the excess dibromopropane gave 53% yield of the alkyne. The alkyne is then dissolved in 45 mL DMSO and to that is added 0.0639 mol sodium azide. The reaction is placed under nitrogen and allowed to stir at room temperature for 18 hours. An equal volume of water was then added followed by extraction with ether, washing of the organic layer with brine, and drying over sodium sulfate. Solvent was removed from the organic layer and flash column chromatography was used to further purify the compound. The azide (6.4 mmol) was then dissolved in 20 mL THF. This solution was transferred by cannula to 60 mL THF containing 57.6 mmol lithium aluminum hydride. Refluxing of the solution continued for 20 hours. The reaction mixture was cooled to 0 C and saturated sodium sulfate was slowly added until CH2OH TBSCl, imid

  • highly stereoselective intramolecular formal 3 3 cycloaddition reactions of vinylogous amides tethered with α β β unsaturated iminiums a formal total synthesis of Gephyrotoxin
    2001
    Co-Authors: Lin-li Wei, Heather M. Sklenicka, Aleksey I. Gerasyuto, Richard P. Hsung
    Abstract:

    To a round bottom flask is added 0.178 mol propargyl alcohol, and 350 mL THF. The reaction is cooled to 0 C followed by addition of 0.196 mol TBSCl, 0.2 mol imidazole, and 0.017 mol DMAP. The reaction is stirred and allowed to come to room temperature. Upon completion by TLC the solvent is removed and column chromatography gave 91% yield of the protected alcohol. The protected alcohol (80.7 mmol) was dissolved in 225 mL THF and HMPA (1.44 mL) as well as 3 mg triphenylmethanol were added. This solution was cooled to –40 C (dry ice/acetone) and 80.7 mmol n-BuLi (2.18 M in hexanes) is added dropwise. After stirring for 30 minutes the reaction is warmed to room temperature. 1,3-dibromopropane (for hexenol) or 1,4dibromobutane (for heptenol) (161.4 mmol) is then filtered through silica and added to the reaction mixture. The reaction was allowed to stir for 2 days at room temperature. Quenching of the reaction was done with dropwise addition of water. THF was removed under reduced pressure, and extracted from ether/water. Removal of solvents from the organic layer followed by distillation of the excess dibromopropane gave 53% yield of the alkyne. The alkyne is then dissolved in 45 mL DMSO and to that is added 0.0639 mol sodium azide. The reaction is placed under nitrogen and allowed to stir at room temperature for 18 hours. An equal volume of water was then added followed by extraction with ether, washing of the organic layer with brine, and drying over sodium sulfate. Solvent was removed from the organic layer and flash column chromatography was used to further purify the compound. The azide (6.4 mmol) was then dissolved in 20 mL THF. This solution was transferred by cannula to 60 mL THF containing 57.6 mmol lithium aluminum hydride. Refluxing of the solution continued for 20 hours. The reaction mixture was cooled to 0 C and saturated sodium sulfate was slowly added until CH2OH TBSCl, imid

Noritaka Chida - One of the best experts on this subject based on the ideXlab platform.