反应详情

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.

1. additionwas then added at a rate
2. temperatureto maintain the temperature at above 125°
3. temperatureThe mixture was refluxed for three and one half hours
4. additionafter the addition
5. temperatureIt was then cooled
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto yield a dark oil, (15 g) which
9. customabsorption in the infrared spectrum at 2250 cm-1
10. customThis intermediate was used without further purification