反応 #323709

反応方程式

phosgene

bicyclooctane

N-butylaminocarbonyl-4-methyl-3-thiophenesulfonamide

→

4-Methyl-3-thiophenesulfonyl isocyanate

溶媒

反応条件

後処理

1. 1
   workup.ADDITIONwas then added at a rate
2. 2
   温度to maintain the temperature at above 125°
3. 3
   温度The mixture was refluxed for three and one half hours
4. 4
   workup.ADDITIONafter the addition
5. 5
   温度It was then cooled
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuo
8. 8
   その他to yield a dark oil, (15 g) which
9. 9
   その他absorption in the infrared spectrum at 2250 cm-1
10. 10
    その他This intermediate was used without further purification

実験手順

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.

出典