Reaktion #323709

Reaktionsgleichung

phosgene

bicyclooctane

N-butylaminocarbonyl-4-methyl-3-thiophenesulfonamide

→

4-Methyl-3-thiophenesulfonyl isocyanate

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas then added at a rate
2. 2
   Temperaturto maintain the temperature at above 125°
3. 3
   TemperaturThe mixture was refluxed for three and one half hours
4. 4
   workup.ADDITIONafter the addition
5. 5
   TemperaturIt was then cooled
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated in vacuo
8. 8
   Sonstigeto yield a dark oil, (15 g) which
9. 9
   Sonstigeabsorption in the infrared spectrum at 2250 cm-1
10. 10
    SonstigeThis intermediate was used without further purification

Vorschrift

A mixture of 18.8 g of N-butylaminocarbonyl-4-methyl-3-thiophenesulfonamide, 0.3 g of 1,4-diaza-[2.2.2.]bicyclooctane and 100 ml of dry xylenes was heated to reflux (136° C.) and 7.4 g of phosgene was then added at a rate to maintain the temperature at above 125°. The mixture was refluxed for three and one half hours after the addition was completed. It was then cooled, filtered and concentrated in vacuo to yield a dark oil, (15 g) which showed absorption in the infrared spectrum at 2250 cm-1. This intermediate was used without further purification.

Quelle