반응 #323709

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phosgene

bicyclooctane

N-butylaminocarbonyl-4-methyl-3-thiophenesulfonamide

→

4-Methyl-3-thiophenesulfonyl isocyanate

용매

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후처리

1. 1
   workup.ADDITIONwas then added at a rate
2. 2
   온도to maintain the temperature at above 125°
3. 3
   온도The mixture was refluxed for three and one half hours
4. 4
   workup.ADDITIONafter the addition
5. 5
   온도It was then cooled
6. 6
   여과filtered
7. 7
   농축concentrated in vacuo
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   기타to yield a dark oil, (15 g) which
9. 9
   기타absorption in the infrared spectrum at 2250 cm-1
10. 10
    기타This intermediate was used without further purification

실험 절차

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.

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