Reaktion #354722

ord-e0f8b1e470004fe393ba43cc7b2afcc4

Lösungsmittel

Reaktionsbedingungen

Temperatur
10°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturWhile cooling
  2. 2
    Filtrationthe precipitate was filtered
  3. 3
    Waschentwice water-washed with 1 liter portions of water
  4. 4
    Sonstigeair-dried
  5. 5
    Sonstigeto give 80.5 g

Vorschrift

While cooling and stirring at 10°C, 76.8 g. (0.50 mole) 2,2-dimethylthiazolidine hydrochloride [preparation described by B. Sweetman et al, J. Med. Chem. 12, 888 (1969)] was added to a mixture of 30 ml isopropanol and 101 g. (1.00 mole) triethylamine. Likewise, 38.0 g. (0.50 mole) of carbon disulfide was gradually added, followed by 45.8 g. (0.25 mole) of anhydrous zinc acetate. After standing overnight at room temperature, the precipitate was filtered, twice water-washed with 1 liter portions of water and air-dried to give 80.5 g. of the yellow product melting at 148° - 153°C (decomp.) and having the following analysis: Found: C, 31.51; H, 4.70%. Calcd for C12H20N2S6Zn: C, 32.04; H, 4.45%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US03943143uspto-grants-1976_03