Reaktion #64342

ord-5032214252f7423c99baac7bb571e4d2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturat reflux for 10 hours
  3. 3
    SonstigeThe solvent was removed by distillation
  4. 4
    Sonstigethe residue was purified by silica gel column chromatography (developing solution: CH2Cl2)

Vorschrift

A mixture of 0.44 g of N-methyl-6-cyano-3,4-dihydro-3-hydroxy-2,2-dimethyl-2H-1-benzopyran-4-carbothioamide, 0.07 g of p-toluenesulfonic acid monohydrate, and 30 ml of toluene was heated at reflux for 10 hours. The solvent was removed by distillation, and the residue was purified by silica gel column chromatography (developing solution: CH2Cl2) to obtain 0.18 g of-N-methyl-6-cyano-2,2-dimethyl-2H-1-benzopyran-4-carbothioamide represented by formula shown below.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05412117uspto-grants-1995_05