2032-75-9Relevant articles and documents
Ortho-spirocarbonates and ortho-spirothiocarbonates: synthesis, functionalization and coupling
Cadoni, Enzo,Perra, Efisio,Fattuoni, Claudia,Bruno, Giuseppe,Cabiddu, Maria G.,De Montis, Stefania,Cabiddu, Salvatore
, p. 2279 - 2284 (2009)
This paper describes a new efficient synthesis of 2,2′-spirobi-(1,3-benzoxathiole) (1), 2,2′-spirobi-(1,3-benzodithiole) (2) and 2,2′-spirobi-(1,3-benzodioxole) (3). Compound 3 has been functionalized by means of metallation reaction followed by electrophilic quenching to give carboxylic acids, aldehydes and alcohols. Furthermore compound 3 was subjected to homo-coupling and its dimeric structure was determined by XRD analysis.
A Traceless Tether Strategy for Achieving Formal Intermolecular Hexadehydro-Diels-Alder Reactions
Smela, Merrick Pierson,Hoye, Thomas R.
supporting information, p. 5502 - 5505 (2018/09/12)
A synthetic strategy formally equivalent to an intermolecular hexadehydro-Diels-Alder (HDDA) reaction is described. Sulfur-based linkers were designed and constructed by joining terminal alkynes or diynes using alkyne thiolate chemistry. The resulting tetraynes and triynes successfully underwent HDDA cyclization and benzyne trapping. Linker removal by reductive desulfurization was uneventful. The strategy was also found suitable for the tetradehydro-Diels-Alder (TDDA) reaction.
One-pot preparation method of 2,2-difluoro-1,3-benzodioxole
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Paragraph 0008; 0011, (2017/08/30)
The invention relates to a one-pot preparation method of 2,2-difluoro-1,3-benzodioxole. The one-pot preparation method of 2,2-difluoro-1,3-benzodioxole is characterized by comprising the following steps: adding piperonyl cyclonene, phosphorus oxychloride and phosphorus pentachloride in a lined polytetrafluoroethylene stainless steel bottle, rising temperature to reflux, ending the reaction when the content of piperonyl cyclonene taken as a raw material is detected to be less than 0.2% by GC, carrying out vacuum rectification on a reaction solution to distill off phosphorus trichloride which is a byproduct and phosphorus oxychloride taken as a solvent; cooling to the temperature of 0 to 5 DEG C after the vacuum rectification is finished, dropwise adding hydrogen fluoride liquid at the vacuum degree of minus 0.1 to minus 0.09MPa, then carrying out heat preservation and releasing the byproduct, namely hydrogen chloride; then dropwise adding a saturated sodium carbonate aqueous solution, adjusting the PH value of the solution to be 6.5 to 7.5, stirring and standing to be stratified, taking an organic layer and distilling to obtain a finished product, namely 2,2-difluoro-1,3-benzodioxole which is colorless and transparent liquid. The one-pot preparation method of 2,2-difluoro-1,3-benzodioxole disclosed by the invention has the advantages of low reaction temperature, high safety and improved yield.