반응 #214522

반응 방정식

naphthol

2-(N-tert-butylsulfamoyl)-4-(2,5-dimethyl-4-sulphophenylazo)-5-methanesulfonamido-1-naphthol

acetonitrile

phosphorus oxychloride

→

2-(N-tert-butylsulfamoyl)-4-(2,5-dimethyl-4-chlorosulfonylphenylazo)-5-methanesulfonamido-1-naphthol

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise at a temmperature below 60° C.
2. 2
   workup.STIRRINGThe mixture was stirred at 60° C. for 3 hours
3. 3
   기타The cyrstals thus-precipitated
4. 4
   여과were collected by filtration
5. 5
   세척washed with 100 ml of acetonitrile

실험 절차

To a solution containing 25 g of the naphthol compound obtained in Step (1) above, 180 ml of acetonitrile and 35 ml of phosphorus oxychloride, 15 ml of N,N-dimethylacetamide was added dropwise at a temmperature below 60° C. with stirring. The mixture was stirred at 60° C. for 3 hours and was poured into 800 ml of ice water. The cyrstals thus-precipitated were collected by filtration and washed with 100 ml of acetonitrile.

출처