Reaktion #1536601

ord-ce32893f45094133ba994ef1c6561a9f

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe excess of isopropanol was removed by distillation under diminished pressure
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in ether
  3. 3
    Filtrationthe ethereal solution was filtered
  4. 4
    SonstigeThe ethereal solution was evaporated under diminished pressure

Vorschrift

To a sample of 5 grams of Example 2B, i.e., 4-neopentyl-3-t-butyl 1,2 dithiole perchlorate, in 50 grams of isopropanol was added 2.5 grams of triethylamine. The excess of isopropanol was removed by distillation under diminished pressure. The residue was dissolved in ether and the ethereal solution was filtered. The ethereal solution was evaporated under diminished pressure to yield 4.3 grams (98% of theory) of 3-isopropoxy-3-t-butyl-4-neopentyl 1,2 dithiole; n.m.r. (CCl4) in ppm, 3.97, 1H singlet (vinyl); 6.18 1H multiplet (isopropoxy); 7.17, 1H doublet (diastereotopic, J=15 cps, neopentyl; 7.88, 1H doublet (diastereotopic, J=15 cps, neopentyl); 8.62, 9H singlet (t-butyl); 8.83, 6H doublet (isopropoxy); and 8.91, 9H singlet (t-butyl).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04190727uspto-grants-1980_02