Reaktion #64347

Reaktionsgleichung

N-ethyl-6-cyano-2,2-dimethyl-2H-1-benzopyran-4-carbamide

Lawesson's reagent

→

N-ethyl-6-cyano-2,2-dimethyl-2H-1-benzopyran-4-carbothioamide

Ausbeute 80.7%

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas refluxed for 1 hour
2. 2
   FiltrationAny insoluble matter was collected by filtration with suction
3. 3
   Waschenwashed with methylene chloride
4. 4
   Sonstigethe solvent was removed
5. 5
   workup.DISTILLATIONby distillation
6. 6
   SonstigeThe residue was purified by silica gel column chromatography (developing solution: CH2Cl2)

Vorschrift

A mixture of 0.14 g of N-ethyl-6-cyano-2,2-dimethyl-2H-1-benzopyran-4-carbamide, 3.45 g of Lawesson's reagent, and 10 ml of benzene was refluxed for 1 hour. Any insoluble matter was collected by filtration with suction and washed with methylene chloride. The mother liquor and the washing were combined, and the solvent was removed therefrom by distillation. The residue was purified by silica gel column chromatography (developing solution: CH2Cl2) to obtain 0.12 g of N-ethyl-6-cyano-2,2-dimethyl-2H-1-benzopyran-4-carbothioamide represented by formula shown below.

Quelle