반응 #1099224

반응 방정식

2-{[4-chloro-2-((E)-{4-[ethyl(2-hydroxyethyl)amino]-phenyl}-diazenyl)-1,3-thiazol-5-yl]methylidene}-1H-indene-1,3(2H)-dione

chlorosulfonic acid

→

2-[{4-[(E)-{4-chloro-5-[(1,3-dioxo-1,3-dihydro-2H-inden-2-ylidene)methyl]-1,3-thiazol-2-yl}diazenyl]phenyl}(ethyl)amino]ethyl Hydrogen Sulfate

용매

THF

반응 조건

후처리

1. 1
   workup.ADDITIONAfter the addition
2. 2
   온도the reaction mixture was heated
3. 3
   온도under reflux for 4 hours
4. 4
   온도to cool to room temperature
5. 5
   workup.STIRRINGstirred overnight
6. 6
   온도After further cooling in an ice bath the formed precipitate
7. 7
   여과was filtered off
8. 8
   세척washed with a little cold THF
9. 9
   기타dried at 40° C. in vacuum

실험 절차

0.5 g (1.07 mmol) 2-{[4-chloro-2-((E)-{4-[ethyl(2-hydroxyethyl)amino]-phenyl}-diazenyl)-1,3-thiazol-5-yl]methylidene}-1H-indene-1,3(2H)-dione were dissolved in 50 ml THF and cooled to 0° C. Then 0.19 g (1.60 mmol) chlorosulfonic acid were added slowly drop by drop with stirring. After the addition was completed, the reaction mixture was heated under reflux for 4 hours, allowed to cool to room temperature and stirred overnight. After further cooling in an ice bath the formed precipitate was filtered off, washed with a little cold THF and dried at 40° C. in vacuum.

출처