反応 #63155

反応方程式

product

N-[(Butylamino)carbonyl]-2-(4,5-dihydro-4-methyl-5-oxo-1,3,4-oxadiazol-2-yl)benzenesulfonamide

DABCO

phosgene

→

subject compound

収率 108.7%

2-(4,5-Dihydro-4-methyl-5-oxo-1,3,4-oxadiazol-2-yl)benzenesulfonyl isocyanate

収率 108.7%

溶媒

反応条件

後処理

1. 1
   workup.ADDITIONwas added portionwise at a rate
2. 2
   温度to maintain a reflux temperature of about 130°-135° C
3. 3
   温度The mixture was refluxed an additional two hours
4. 4
   ろ過filtered
5. 5
   濃縮the filtrate was concentrated in vacuo

実験手順

A suspension of 8 g of the product of Example 7 and 0.4 g of DABCO in 90 ml of xylenes was heated under N2 at 130°-135° C. while 1.8 ml of phosgene was added portionwise at a rate to maintain a reflux temperature of about 130°-135° C. The mixture was refluxed an additional two hours, cooled under N2 to room temperature, filtered, and the filtrate was concentrated in vacuo to yield 6.9 g of the subject compound as a crude oil.

出典